Sciencemadness Discussion Board

Benzyl Alcohol -> Benzaldehyde via Silica Gel Supported Jones Reagent

Hilski - 18-9-2006 at 14:35

Anyone ever try this? Seems way too easy to be true.


Representative Procedure

Dry silica gel (5 g) was placed in a 100-mL round-bottom flask containing a magnetic stirring bar and fitted with a rubber septum. Jones reagent (1.5mL, 12 mmol) was added slowly from a syringe to the vigorously stirred silica gel. After complete addition of the reagent, stirring continued until a free-flowing orange powder was obtained (less than 5 min). Methylene chloride (25 mL) was added to the above flask. A solution of benzyl alcohol 1a (396 mg, 3.66 mmol) in methylene chloride (5 mL) was added slowly from a syringe through the rubber septum to the stirred heterogeneous mixture. The orange SJR turned dark green/brown immediately. After complete disappearance of the starting benzyl alcohol as indicated by TLC (10 min), the reaction mixture was filtered through a sintered glass funnel, the solid residue was washed with methylene chloride (75 mL) and the washings were added to the filtrate. Solvent was removed from the solution under vacuum to produce a colorless oil (331.6 mg, 85.3% yield) which was pure benzaldehyde according to NMR and IR data.

More details from Erowid:

http://www.erowid.org/archive/rhodium/chemistry/alcohol2alde...

-Hilski

Hilski - 20-9-2006 at 12:50

Seems the answer was right here all along. Or at least something close. I suppose that as long as no water is allowed into a Jones-type oxidation, then it should work OK?

https://sciencemadness.org/talk/viewthread.php?tid=5839

The last 4 or 5 posts in that thread is a discussion about variations of a Jones oxidation.

Quote: "Use of CrO3 with NaHSO4.H2O (Sodium Bisulfate Monohydrate) in 1:1:1 ratio will give you bezaldehyde by 95% yield. ( Im still using it myself,trust it)"

'Tis worth looking into I would say. I wonder if dichromate would also work in this case as well?

redox - 15-7-2011 at 17:34

I have performed this exact synthesis before, and it works like a dream. Isolation of product is trivial, and the whole reaction is clean and easy.

mario840 - 15-7-2011 at 21:56

better is PCC (pyridinum chlorochromate) , easy synth reagent and easy synthesis oxidize

redox - 16-7-2011 at 08:01

Quote: Originally posted by mario840  
better is PCC (pyridinum chlorochromate) , easy synth reagent and easy synthesis oxidize


The only problem with PCC is that it is much more difficult to acquire than silica gel.

simba - 21-7-2011 at 16:01

Why not use calcium/sodium hypochlorite? The link below says it is possible and gives 98% yields, though it says that benzyl alcohol is the only (or one of the few) primary alcohol(s) that can get oxidized into an aldehyde using hypochlorites.

http://www.erowid.org/archive/rhodium/chemistry/ether2ester.hypochlorite.html

redox - 21-7-2011 at 17:48

I would love to try this, but the synthesis calls for acetonitrile, which I cannot make nor purchase. I wonder if a different compound could be substituted in its place....

Melgar - 21-7-2011 at 18:43

Does anyone have experience with the procedure in the attached pdf? It uses iodine radicals to oxidize benzyl alcohol to benzaldehyde, then the iodide is oxidized back to iodine by molecular oxygen. Seems pretty easy, especially if you have access to a source of pure oxygen.

Attachment: benzaldehyde.pdf (146kB)
This file has been downloaded 1364 times

simba - 21-7-2011 at 19:25

Quote: Originally posted by redox  
I would love to try this, but the synthesis calls for acetonitrile, which I cannot make nor purchase. I wonder if a different compound could be substituted in its place....


I'm pretty sure acetonitrile is just a solvent they decided to use for adding the menthol dropwise, since pure menthol is a waxy solid. But you don't need it for working with benzyl alcohol since its a liquid already.

redox - 22-7-2011 at 04:44

In that case, I will be attempting this procedure with benzyl alcohol post-haste. :)

simba - 5-8-2011 at 18:52

Ok I tried today the oxidation of benzyl alcohol with calcium hypochlorite and I can only classify it as 'disastrous success'.

I mixed 155g of 65% calcium hypochlorite from bleaching powder with 600ml of water and 110g of benzyl alcohol. The reaction went smooth in the beginning, with no heating evolved, and I could smell benzaldehyde being formed...then after 2 hours I heard an explosion. I went to see what happened and my laundry room was entirely painted with spills from the reaction mixture and the smell was so strong I could barely breath.

It seems the reaction spontaneously boiled to the point of exploding in a volcanic stream of benzaldehyde. I just want to know what the fuck happened...I know calcium hypochlorite is known for undergoing self heating, but I added just the enough for the reaction...does anyone have a clue of what happened?

DJF90 - 5-8-2011 at 20:57

For a start, the paper claims acetic acid is required for the oxidation. Secondly, the paper runs the reaction in an ice bath. And finally, your volume of solvent is far off if a direct scale-up is attempted. Perhaps you should try new reactions following the experimental procedure outlined in the reference and on a small scale to avoid such dangerous situations and the large waste of materials.

Nicodem - 6-8-2011 at 02:49

Quote: Originally posted by shivas  
I mixed 155g of 65% calcium hypochlorite from bleaching powder with 600ml of water and 110g of benzyl alcohol.

...then after 2 hours I heard an explosion. I went to see what happened and my laundry room was entirely painted with spills from the reaction mixture and the smell was so strong I could barely breath.

Sorry for being offensive, but I just can't help not saying: "What an idiot!"
How could you expect anything else but a runaway could happen by doing an oxidation on a one mol scale under totally uncontrolled conditions? I have to restrain myself of not telling you what I think of such a behavior. Could you have done this in any more stupid way? Only by doing it on 10 mol!
Well, at least you had the luck of not being present at the moment of the accident.

TO ALL: Don't scale up exothermic reactions without process research!

I can't believe these things still happen after so many safety warnings. Does nobody ever UTFSE by using keywords like: runaway, mishap, safety, accident, scale up...

http://www.sciencemadness.org/talk/viewthread.php?tid=3698

simba - 6-8-2011 at 07:14

Yeah, I can only agree about that, epic idiocy, and nothing more. I could try to justify it, but its just unjustifiable really, I don't even know what I was thinking at the time I made that post, I guess I was just knocked out by the strong smell of benzaldehyde in my house.

But well, what does not kill you...makes you learn.

DJF90 - 6-8-2011 at 07:28

Its not the fact you made the post thats the problem, and so you cannot blame the smell of benzaldehyde. What you did was really inconsiderate, running a new reaction on the molar scale without even following the same procedure that was used. The large amount of water used in the paper is NECESSARY as there is a large amount precipitate formed during the reaction, which may prevent/hinder magnetic stirring. Towards the end of the reaction all of this precipitate is redissolved. I'd suggest overhead stirring for anything over about 100mmol.

simba - 6-8-2011 at 08:17

Quote: Originally posted by DJF90  
Its not the fact you made the post thats the problem, and so you cannot blame the smell of benzaldehyde. What you did was really inconsiderate, running a new reaction on the molar scale without even following the same procedure that was used. The large amount of water used in the paper is NECESSARY as there is a large amount precipitate formed during the reaction, which may prevent/hinder magnetic stirring. Towards the end of the reaction all of this precipitate is redissolved. I'd suggest overhead stirring for anything over about 100mmol.


The reason I feel stupid about that post is just because I said I had no clue of what had happened. I was already expecting some highly exotermic reaction, but I could feel the smell of benzaldehyde and no rise in temperature, so I just assumed nothing would happen thereafter, I was very wrong then.

MolecularArchitect - 10-8-2011 at 08:45

@redox Do you have any experience with scaling up the procedure herein mentioned?

redox - 10-8-2011 at 13:39

Quote: Originally posted by MolecularArchitect  
@redox Do you have any experience with scaling up the procedure herein mentioned?


Somewhat. I performed the synthesis on a two-times scale, which was about 7.32 mmol benzyl alcohol (some [read: most] might still consider this small scale :cool: ). Once I get some more silica gel, I will try it again on a .25 mol scale or near that.


[Edited on 10-8-2011 by redox]

MeSynth - 20-8-2011 at 12:26

After doing a bit of math I discovered that if you wanted to scale this up say... 1000x ( in order to produce 300ml of benzaldehyde ) your going to need A LOT of silica gel... if you found a good supplier of silica gel then it would be ok the next problem is the large flask you would need. Glass punch bowl? or one of those glass water jugs that Chunk drops in The Goonies.

redox - 21-8-2011 at 06:50

Quote: Originally posted by MeSynth  
After doing a bit of math I discovered that if you wanted to scale this up say... 1000x ( in order to produce 300ml of benzaldehyde ) your going to need A LOT of silica gel... if you found a good supplier of silica gel then it would be ok the next problem is the large flask you would need. Glass punch bowl? or one of those glass water jugs that Chunk drops in The Goonies.


I think its clear that this synthesis was not designed to be scaled up. Plus, who needs 300mL of benzaldehyde? :)

It would be interesting to do some experiments to see if the ratio of silica gel to Jones' Reagent could be lowered, to save some of the valuable silica gel.

Does anyone have a good source for the gel? My only source was ~55$ for 300g silica gel! Of course, this was for very fine mesh, I think 0.4 um - 0.63um, or something like that.

MeSynth - 21-8-2011 at 09:11

Quote: Originally posted by redox  
Quote: Originally posted by MeSynth  
After doing a bit of math I discovered that if you wanted to scale this up say... 1000x ( in order to produce 300ml of benzaldehyde ) your going to need A LOT of silica gel... if you found a good supplier of silica gel then it would be ok the next problem is the large flask you would need. Glass punch bowl? or one of those glass water jugs that Chunk drops in The Goonies.


I think its clear that this synthesis was not designed to be scaled up. Plus, who needs 300mL of benzaldehyde? :)

It would be interesting to do some experiments to see if the ratio of silica gel to Jones' Reagent could be lowered, to save some of the valuable silica gel.

Does anyone have a good source for the gel?


Would it be possible to lessen the amount of silica gel used? Why don't you find out how the reaction works, tell us =P, and then we can answer your question.

redox - 21-8-2011 at 11:37

Quote: Originally posted by MeSynth  
Quote: Originally posted by redox  
Quote: Originally posted by MeSynth  
After doing a bit of math I discovered that if you wanted to scale this up say... 1000x ( in order to produce 300ml of benzaldehyde ) your going to need A LOT of silica gel... if you found a good supplier of silica gel then it would be ok the next problem is the large flask you would need. Glass punch bowl? or one of those glass water jugs that Chunk drops in The Goonies.


I think its clear that this synthesis was not designed to be scaled up. Plus, who needs 300mL of benzaldehyde? :)

It would be interesting to do some experiments to see if the ratio of silica gel to Jones' Reagent could be lowered, to save some of the valuable silica gel.

Does anyone have a good source for the gel?


Would it be possible to lessen the amount of silica gel used? Why don't you find out how the reaction works, tell us =P, and then we can answer your question.


The reaction works by forming an intermediate chromate ester which is cleaved, giving an aldehyde and a less oxidized oxochromium acid.

I personally don't understand why silica gel lessens the activity of and raises the selectivity of the Jones' reagent. Does anybody out there in the internet know?

MeSynth - 21-8-2011 at 14:09

Silica gel used in the oxidation reactions, as solid support, was MN-Kieselgel 60 (0.04–0.063mm mesh size) supplied by Fisher Scientific.

------------------------------Taken from the link in the original post

Used as a solid support. Maybe plain old glass dust would work.

redox - 21-8-2011 at 14:40

Quote: Originally posted by MeSynth  
Silica gel used in the oxidation reactions, as solid support, was MN-Kieselgel 60 (0.04–0.063mm mesh size) supplied by Fisher Scientific.

------------------------------Taken from the link in the original post

Used as a solid support. Maybe plain old glass dust would work.


Well, it is obviously a solid support. Dust won't work. Dust is made up mostly of dust, hair, and skin cells. Silica gel is very porous with an enormous surface area, which adsorbs (or absorbs? not sure) the Jones reagent. My question was why it modifies the activity of the Jones Reagent.

questions - 26-8-2011 at 18:52

Our friend "cyclonknight" described an attractive process for making benzaldehyde from cinnamon oil by slowly dripping the cinnamon oil into the already boiling water with dissolved NaOH at around a PH of 12 to 13.
What I dont understand is that on the wikipedia they say that benzaldehyde is converted into two other chemicals when exposed to highly concentrated NaOH, and I quote

"Benzaldehyde undergoes disproportionation upon treatment with concentrated alkali (Cannizzaro reaction): one molecule of the aldehyde is reduced to the corresponding alcohol and another molecule is simultaneously oxidized to sodium benzoate."

So if the cinnamon oil is being converted to benzaldehyde, and is steam disstilled out, why isn't the benzaldehyde being converted into other products as described by the wikkipedia?

redox - 27-8-2011 at 08:01

Quote: Originally posted by questions  
Our friend "cyclonknight" described an attractive process for making benzaldehyde from cinnamon oil by slowly dripping the cinnamon oil into the already boiling water with dissolved NaOH at around a PH of 12 to 13.
What I dont understand is that on the wikipedia they say that benzaldehyde is converted into two other chemicals when exposed to highly concentrated NaOH, and I quote

"Benzaldehyde undergoes disproportionation upon treatment with concentrated alkali (Cannizzaro reaction): one molecule of the aldehyde is reduced to the corresponding alcohol and another molecule is simultaneously oxidized to sodium benzoate."

So if the cinnamon oil is being converted to benzaldehyde, and is steam disstilled out, why isn't the benzaldehyde being converted into other products as described by the wikkipedia?


Questions, you have posted this message in at least four places. Crossposting is not acceptable and it is confusing.

Please do not crosspost again.

chucknorris - 20-4-2012 at 12:28

Quote: Originally posted by Hilski  
Dry silica gel (5 g) was placed in a 100-mL round-bottom flask containing a magnetic stirring bar and fitted with a rubber septum. Jones reagent (1.5mL, 12 mmol) was added slowly from a syringe to the vigorously stirred silica gel. After complete addition of the reagent, stirring continued until a free-flowing orange powder was obtained (less than 5 min). Methylene chloride (25 mL) was added to the above flask. A solution of benzyl alcohol 1a (396 mg, 3.66 mmol) in methylene chloride (5 mL) was added slowly from a syringe through the rubber septum to the stirred heterogeneous mixture. The orange SJR turned dark green/brown immediately. After complete disappearance of the starting benzyl alcohol as indicated by TLC (10 min), the reaction mixture was filtered through a sintered glass funnel, the solid residue was washed with methylene chloride (75 mL) and the washings were added to the filtrate. Solvent was removed from the solution under vacuum to produce a colorless oil (331.6 mg, 85.3% yield) which was pure benzaldehyde according to NMR and IR data.


Is it really necessary to use such a huge amounts of DCM to dissolve all that stuff? I mean like, when you want to use 39.6g of benzyl alcohol which will yield no more than ~30 grams of benzaldehyde, you would have to use hegemonic THREE LITERS of DCM for that??

bamboula - 1-5-2014 at 05:12

Quote: Originally posted by DJF90  
For a start, the paper claims acetic acid is required for the oxidation. Secondly, the paper runs the reaction in an ice bath. And finally, your volume of solvent is far off if a direct scale-up is attempted. Perhaps you should try new reactions following the experimental procedure outlined in the reference and on a small scale to avoid such dangerous situations and the large waste of materials.


sorry for bumping an old thread
DJF90 can you tell me where i can find this paper ?
thx alot

SM2 - 1-5-2014 at 07:36

Nicodem,

Your SmartAs they come. Just don't understand the reasons behind your anti-social aspects, exhibited on our SM board. You are a genius, no doubt. Now just be nice here. Find people who truly deserve to be taunted and abused. Like the evil, dysfunctional Fed DOJ, who ruin people's lives every day with their seemingly unlimited, unchecked power. Fed prosecutors can virtually prosecute any us citizen they want, regardless of merit. (off topic, sorry). Other than that, you are a tremendous asset to SM.

SIMBA: Easy-Peazy. Just take a nice slog of bleach, and add a little NaOH (we want to keep the pH up a bit). Mag stir, and slowly add your benzyl alcohol. It is simple, uncomplicated, fast, and very forgiving. Sep it. I'd distill, but you don't actually have to. The RXN is very clean, and the mechanism is analogous to using hypochlorite (aq) to form aldehydes from some amino acids. Like phenylacetaldehyde from phenylalanine.

Nicodem probably knows a hell lot more if your really interested. Just remember, someone of his caliber will not accept any sloppy thinking. Carefully proof read your question, do as much research as you can, and if you don't know something, admit it. Supply all the info you can garner. In this way, experts are able, at their discretion, to give you their best answer without having to waste their precious time muddling through a bunch of gob dilly gook.

Dr.Bob - 1-5-2014 at 07:49

Using solid supported reagents does require lots of solvent, but in many cases the solvents and/or solid supports can be reused. Often simply washing the used silica gel with new reagents will reactivate it and it can be reused a few times at least. As well the DCM can be easily rotovap'd or distilled off and reused many times. So they are not perfect, but easily scalable by either continous flow or small batches and reusing the materials. Many other solid supported reagents can be reactivated (but not all). But they can allow for very simple reactions at times.

And people here should head the warning that scaling up reactions should be done slowly. If the procedure says 1 g, try it first, then try 10 g then go to 100 g. I have seen several large messes made in the same manner. Also pay attention to the order of addition. As noted by SM2, sometimes if you mix certain things first, the reaction will be more easily controlled, often the paper specifies a specific order, and I have seen many people ignore it to bad results. Unless you are familiar with a reaction, the best way to reproduce it is the exact way it was done before, making changes without reason will often give bad results. It is not always possible to redo exactly, but the closer the better. Few people cool a reaction in ice just because, so if they say to do it, there is likely a reason.

bamboula - 1-5-2014 at 09:02

Quote: Originally posted by SM2  
Nicodem,

Your SmartAs they come. Just don't understand the reasons behind your anti-social aspects, exhibited on our SM board. You are a genius, no doubt. Now just be nice here. Find people who truly deserve to be taunted and abused. Like the evil, dysfunctional Fed DOJ, who ruin people's lives every day with their seemingly unlimited, unchecked power. Fed prosecutors can virtually prosecute any us citizen they want, regardless of merit. (off topic, sorry). Other than that, you are a tremendous asset to SM.

SIMBA: Easy-Peazy. Just take a nice slog of bleach, and add a little NaOH (we want to keep the pH up a bit). Mag stir, and slowly add your benzyl alcohol. It is simple, uncomplicated, fast, and very forgiving. Sep it. I'd distill, but you don't actually have to. The RXN is very clean, and the mechanism is analogous to using hypochlorite (aq) to form aldehydes from some amino acids. Like phenylacetaldehyde from phenylalanine.

Nicodem probably knows a hell lot more if your really interested. Just remember, someone of his caliber will not accept any sloppy thinking. Carefully proof read your question, do as much research as you can, and if you don't know something, admit it. Supply all the info you can garner. In this way, experts are able, at their discretion, to give you their best answer without having to waste their precious time muddling through a bunch of gob dilly gook.


SM2 what are the yield with this reaction ?
do you have some reference?
also do you know where can i find the paper i mentionned above ?
thx

SM2 - 1-5-2014 at 12:17



CLIP...SM2 what are the yield with this reaction ?
do you have some reference?
also do you know where can i find the paper i mentioned above ?---CLIP



It's been a long time, just no time any more even for simple experiments it seems, and can't even get you the reference off hand. BUT, I do remember doing it several times, and yield seemed almost quantitative, especially when taking MW's into account.

It's simple and difficult to fuck up. Take maybe 32oz bleach (PLAIN, no added anything), and if you can find the 10% stuff, that's even better. Stir in a teaspoon of NaOH. Room temperature for everything seems to work fine. Drop in your polytef coated magnet, and center, etc. Get a nice stir going. Just a 1" tornado on top is sufficient. Use a sep to add your alcohol. First, let it drip in for a few minutes. You can definitely increase the rate fairly rapidly, but just monitor the temp. Warm is OK. If it's getting hot, stop flow. Part of the runaway with the HTH method is also due to the aldehyde reacting with some inerts in the 65% or so, Calcium Hypochlorite granules, and at high concentration, with an abduct then playing a 2ndary role. It reduces yields, and is unpredictable and dangerous, IMO. But I am very conservative-a true coward in some respects if there is any chance of run away. I guess my worst nightmare might be if I had to distill methyl nitrate or tetranitromethane, nitrogen trichloride, chlorine dioxide. Ugh (sHuTtEr!). The original paper used HTH, and filtered the solution. It also used methanol as well if I'm not mistaken. Just Go with the excess bleach, keep it alkaline, get a good stir going, and you'll be done in 20-30 minutes. When done in this manner, it is very forgiving, with consistently high yields with no worries. Also, the aldehyde seems stabilized somehow by a small amount of perhaps a scavenger formed

If I may be so bold, would you mind explaining what your plans are for the benzaldehyde? It's such a cheap chemical, and unless you have nefarious plans for it's usage, it's probably just easier to just fill out the DEA form and buy the pure stuff cheaply. Unless this is just pilot scale. It all depends on how much you need.

You also can make it by stirring in some nano antease TiO2 into a cup of toluene, exposed to an ordinary black light while bubbling humid air through the mix with a lava stone bubble disperser, and mag stirrer. The TiO2 forms a gap when exposed to certain band widths of UVA. -OH anions will be formed on the TiO2 (water is necessary to form the hydroxyl). This too is very clean, but takes quite a bit longer. The amount of catalyst is a factor, as is the intensity of the UVA. Too much TiO2, and your wasting light by reflecting it back out.

About drugs, DEA, if your not doing anything illegal with your goods, there is nothing to worry about. Believe me, they have almost ingenious ways of knowing when one has crossed that line. It's just not worth it. And if you did succeed in making breaking bad, you'd get busted selling the shit. And selling that shit is unethical as hell. If you want to experiment on a very small level just for your self, I guess the harm to society is not so great.

One thing I absolutely can not stand, the OVERBLOWN, blown out of proportion mountain out of a molehill of contamination worries hysteria. It is unfounded, and untrue, both in spirit, and in most practical ways. Saying a house needs a level of clean up you'd expect maybe if asbestos needles covered in plutonium dust was sprinkled everywhere, with bottles of tetradioxin saturating the carpet.. What an over blown over reaction. I think people who engage in this sort of work for our federal government, are largely the Chuck Norris type, who feel they are somehow sexy and important. They are actually delusional, and buy in to the party line just as the audience for any N. Korean Kim Jung Shit. The Federal Govt is broken, and beyond fixing. Sure, there are some good employees in fed jobs, but every federal worker, including every corrupt politician and policeman. Every "Special Agent" man - they are ALL 2nd class citizens. You see, they are public servants. OK rant over, sorry, someone indeed DID pee in my corn flakes today!








[Edited on 2-5-2014 by SM2]

bamboula - 7-5-2014 at 05:53

Quote: Originally posted by SM2  


CLIP...SM2 what are the yield with this reaction ?
do you have some reference?
also do you know where can i find the paper i mentioned above ?---CLIP



It's been a long time, just no time any more even for simple experiments it seems, and can't even get you the reference off hand. BUT, I do remember doing it several times, and yield seemed almost quantitative, especially when taking MW's into account.

It's simple and difficult to fuck up. Take maybe 32oz bleach (PLAIN, no added anything), and if you can find the 10% stuff, that's even better. Stir in a teaspoon of NaOH. Room temperature for everything seems to work fine. Drop in your polytef coated magnet, and center, etc. Get a nice stir going. Just a 1" tornado on top is sufficient. Use a sep to add your alcohol. First, let it drip in for a few minutes. You can definitely increase the rate fairly rapidly, but just monitor the temp. Warm is OK. If it's getting hot, stop flow. Part of the runaway with the HTH method is also due to the aldehyde reacting with some inerts in the 65% or so, Calcium Hypochlorite granules, and at high concentration, with an abduct then playing a 2ndary role. It reduces yields, and is unpredictable and dangerous, IMO. But I am very conservative-a true coward in some respects if there is any chance of run away. I guess my worst nightmare might be if I had to distill methyl nitrate or tetranitromethane, nitrogen trichloride, chlorine dioxide. Ugh (sHuTtEr!). The original paper used HTH, and filtered the solution. It also used methanol as well if I'm not mistaken. Just Go with the excess bleach, keep it alkaline, get a good stir going, and you'll be done in 20-30 minutes. When done in this manner, it is very forgiving, with consistently high yields with no worries. Also, the aldehyde seems stabilized somehow by a small amount of perhaps a scavenger formed

If I may be so bold, would you mind explaining what your plans are for the benzaldehyde? It's such a cheap chemical, and unless you have nefarious plans for it's usage, it's probably just easier to just fill out the DEA form and buy the pure stuff cheaply. Unless this is just pilot scale. It all depends on how much you need.

You also can make it by stirring in some nano antease TiO2 into a cup of toluene, exposed to an ordinary black light while bubbling humid air through the mix with a lava stone bubble disperser, and mag stirrer. The TiO2 forms a gap when exposed to certain band widths of UVA. -OH anions will be formed on the TiO2 (water is necessary to form the hydroxyl). This too is very clean, but takes quite a bit longer. The amount of catalyst is a factor, as is the intensity of the UVA. Too much TiO2, and your wasting light by reflecting it back out.

About drugs, DEA, if your not doing anything illegal with your goods, there is nothing to worry about. Believe me, they have almost ingenious ways of knowing when one has crossed that line. It's just not worth it. And if you did succeed in making breaking bad, you'd get busted selling the shit. And selling that shit is unethical as hell. If you want to experiment on a very small level just for your self, I guess the harm to society is not so great.

One thing I absolutely can not stand, the OVERBLOWN, blown out of proportion mountain out of a molehill of contamination worries hysteria. It is unfounded, and untrue, both in spirit, and in most practical ways. Saying a house needs a level of clean up you'd expect maybe if asbestos needles covered in plutonium dust was sprinkled everywhere, with bottles of tetradioxin saturating the carpet.. What an over blown over reaction. I think people who engage in this sort of work for our federal government, are largely the Chuck Norris type, who feel they are somehow sexy and important. They are actually delusional, and buy in to the party line just as the audience for any N. Korean Kim Jung Shit. The Federal Govt is broken, and beyond fixing. Sure, there are some good employees in fed jobs, but every federal worker, including every corrupt politician and policeman. Every "Special Agent" man - they are ALL 2nd class citizens. You see, they are public servants. OK rant over, sorry, someone indeed DID pee in my corn flakes today!








[Edited on 2-5-2014 by SM2]


lol thank you SM2

i just need a small quantity of it (50 ml) and since i had a small bottle of benzyl alcohol laying around i thought i could synth some benzaldehyde since it's impossible to find where i live :)

Fantasma4500 - 21-5-2014 at 05:11

about calcium hypochlorite
i recall long time back i read about a guy who was making a guide on 'how to KClO3' or something similar
he used both NaClO and boiled it down, aswell as Ca(ClO)2 however when he used the calcium hypochlorite he had a smaller explosion, it was later determined that NCl3 was the cause

Ca(ClO)2 --- consider NCl3 formation!!

Nicodem - 22-5-2014 at 11:08

Quote: Originally posted by Antiswat  
Ca(ClO)2 --- consider NCl3 formation!!

Wow! He achieved a nuclear reaction by simply boiling down a calcium hypochlorite solution? I wander if it was calcium, chlorine or oxygen that transmutated?

Fantasma4500 - 10-6-2014 at 10:22

Yes!
or well i guess?
dont think he even started boiling it down, he just left it to dissolve in a litre of water and then it just went boom
as something explosive could be generated in situ it should be considered