Sciencemadness Discussion Board - What reagent would you like to see an illustrated guide for?

What reagent would you like to see an illustrated guide for?

len1 - 28-7-2008 at 19:02

Im looking for new syntheses to perform. If you would like to see an illustrated procedure demonstrated for a useful chemical reagent I would gladly consider writing it. Essentially Im looking for chemical reagents, which are useful, not instantly availale, whose procedure for manufacture is lacking in standard texts (in detail, purity analysis, kinetics etc.), is not drug related. CS2, SO3, Na were perfect past examples - have you any ideas of some more?

[Edited on 29-7-2008 by len1]

octave - 28-7-2008 at 19:49

Aldol condensations! Many useful chemicals can be prepared from this process. Though I cannot think of any chemical right off the bat I would love to have a pictorial of this reaction mechanism.

[Edited on 28-7-2008 by octave]

Magpie - 28-7-2008 at 20:22

I think there must be quite a few difficult to obtain reagents that are normally made on an industrial scale and which do not have readily available laboratory methods. I think those you have already mentioned fit that description. Two more that come immediately to mind are phosphorus and CCl4. In time I'm sure I can think of some more.

Also consider the reductants sodium borohydride and lithium aluminum hydride. And the Lewis acid AlCl3. There are also some on this board who would just like to make con H2SO4 without going thru SO3.

Edit: And my favorite, pyridine.

[Edited on 28-7-2008 by Magpie]

UnintentionalChaos - 28-7-2008 at 20:26

Well, Sauron has detailed Carbon tetrachloride quite a bit, but an illustrated guide would be excellent.

I'm sure there'd be an audience for phosphorus, although I wouldn't blame you for shying away from it due to a number of less than savory uses...

You could always tackle hydrazine...useful for precious metals reprocessing and syntheses such as luminol among other things.

EDIT: Magpie beat me to the posting. AlCl3 and borane/borohydrides would also be great.

[Edited on 7-28-08 by UnintentionalChaos]

kclo4 - 28-7-2008 at 20:32

Personality I think a Ketene lamp would be really cool. Perhaps it isn't the hardest thing, but I've never seen a real one and eventually I would like to make one. there is always a setup for it and a sketched picture of the lamp, but never the real thing. Plus, ketene seems like a very useful chemical. Mostly because it can be used in place of Ac2O or make Ac2O from GAA. Ketene is pretty dangerous, but I think making it and using it would be a lot safer then phosphorous and a few other chemicals.

Magpie - 28-7-2008 at 20:32

I thought about hydrazine myself, but I think Mr Anonymous has given us the procedure in a thread on this board, although it is not as facile as an illustrated guide would be. Also, a synthesis for hydrazine sulfate does exist in Inorganic Synthesis, volume I.

kilowatt - 28-7-2008 at 20:35

Some very useful reagents that come to mind are thionyl chloride, nitrosyl chloride, PCl5. Even nitrites like NaNO2 don't seem to have many good lab synthesis methods out there. Precious metal salts and acids are good too. Borate esters are another good one.

kclo4 - 28-7-2008 at 20:48

Mentioning Precious metals, How about an extraction of Pt/Pd from catalytic converters? or perhaps a decent Nickel Catalyst and a demonstration of what they can do?
Not to sure how many uses it has, and its not really that hard to make but I've read a few things on some of them and lately I've been pretty interested in them. I've been dissolving some nickel to try it out with something.

They seem to have pretty good potential.
http://www.erowid.org/archive/rhodium/chemistry/urushibara.h...
Here is a bad example of what one can use them for :S
http://designer-drug.com/pte/12.162.180.114/dcd/chemistry/am...

DJF90 - 28-7-2008 at 23:53

Reducing agents like LAH and NaBH would be great! How about nitric acid from ammonia? And thionyl chloride, without using SO3... Wikipedia states that the reaction SO2 + Cl2 + SCl2 => 2SOCl2 is one method, which i think would probably more easily achieved for the home chemist than the SO3 methods. Maybe also preparation of sodium/potassium cyanide, as cyanide salts can be rather useful in organic chemistry, forming nitriles and the like... Other possibilities include making some sort of apparatus for catalytic hydrogenation, but using hydrogen produced from a reaction like 6NaOH + 2Al => 2NaAlO3 + 3H2, and finding some way of getting the hydrogen to a pressure of 3-10 atm or higher. "Freebase" hydrazine is a good idea, as azides could also be formed by reacting with a nitrite.

Personally some inverstigation into the SOCl2 reaction I posted or LAH/NaBH would be preferred

Picric-A - 29-7-2008 at 01:05

could you show some simple processes used in organic chemicstry for begginers?
eg. fisher esterification, dehydrogenation etc...
good luck with it!
Picric-A

YT2095 - 29-7-2008 at 01:11

personally I would love to seea Diphenyl Oxalate synth using Phenol and oxalic acid as precursors.
maybe via transestrification of diethyl oxalate (that you would also make).

chromium - 29-7-2008 at 02:01

Here are some that come to mind and are not stated by others: Making soluble relatively pure salts of chromium and nickel from stainless steel. Route to phenol starting from turpentine. Making benzene from something better available than benzoates.Use of ion exchange resins to make dilute acids from salts especially if electrolytic or some other easy regeneration of exchangers is possible. Electrolytic chlorine generator which can actually be used for chlorinations.

[Edited on 29-7-2008 by chromium]

stoichiometric_steve - 29-7-2008 at 03:36

LAH please

Klute - 29-7-2008 at 04:57

A low-pressure hydrogenation apparatus is a good idea, I'm starting to make a fewplans on making on to go up to 3 atm. Although it could be easily made from stainless steel, a thick hydrogenation bottle, etc, there are safety issues that need great attention, welding must be done very carefully and I guess there are alot of construction considerations.

With such an apparatus, catalysts like raney nickel (which usually performs very bad a atm pressures), Cu, etc could be very usefull for a great number of reductions.

Organic sulfonic chlorides, from the sulfonic acid and S2Cl2, for example, or chlorination of alkyl thiosulfates or sulfides could be very interesting too.
These could lead to preparation of safer alkylating agents, by reacting them with alcohols, which I think are a constant 'graal'

. Sulfonates could also enable one to perform various displacements.
Trialkylphosphates, from P2O5, or POCl3 from P2O5, etc all could be very usefull and a certain challenge (especially the oxychloride)

I think it's extremly generous on your part to ask memebers of the forum what they would like to see being done!

What ever your futur plans, good luck with it!

woelen - 29-7-2008 at 10:52

A suggestion for len1 would be to add a synth, which also can be done by the moderately equipped home chemist. Chemicals requiring such intermediate apparatus and skills can still be very interesting for the average home chemist. Some to name:
- vanadyl salts like VOSO4.xH2O from pottery grade V2O5
- titanium salts from the metal and easy to obtain acids (e.g. TiCl3)
- luminol from naphthalene, phthalic acid or phthalic anhydride

len1 - 29-7-2008 at 14:44

Thank you very much for your suggestions. Surprisingly the list of preliminarily ideas I jotted down got almost completely covered - CCl4, NaCN, NaN3 etc - so I was thinking on the right track. Some of the suggestions I have'nt thought of at all and will have to read up on, such as what Klute posted. Other things I thought you could readily buy, such as LiAlH4 and AlCl3 - ill have to ring up. Thank you

DJF90 - 29-7-2008 at 14:55

Readily buy LiAlH4?? and where abouts do you live

Ozone - 29-7-2008 at 16:21

I'm with YT on the phenyl oxalates:

Oxalyl chloride and 2,4-dinitrophenol to give DNPO. The DNP we can do, the oxalyl chloride is a bit trickier. Of interest, oxalyl chloride (which Sauron has discussed quite a bit) can be directly oxidized with H2O2 in the presence of a fluorescent dye (i'm using perylene and rhodamine 6G) to yield chemiluminescence.

The PClx needed to make the oxalyl chloride would make this an interesting (if intensive) multi-step process that yields a rather nice chemiluminescent compound.

I have been making these (DNPO, TCPO) from oxalyl chloride and could document the procedure if anyone is interested.

Let's see, what else... Diborane, definitely. Anything with NaK. Reformatsky? LDA enolate formation. Sodamide (maybe not such a good idea, these days). Diazomethane. Magic acid. Some reactions using PTC to enable classical reactions in water. Ionic liquids.

Cheers,

O3

ordenblitz - 29-7-2008 at 17:54

Len.. I was thinking that since your very adept at manufacturing apparatus for chemical reactions, like your sodium cell, in my opinion it would be far more entertaining for the audience for you to stay with things that require skill in that area. The hydrogenation apparatus that Klute suggested or the ketene lamp that kclo4 proposed would be such a challenge. Anyone of us can toss some stuff in a flask and stir. The things that you build are quite amazing.

Regards,

Ord

Magpie - 29-7-2008 at 18:10

I second ordenblitz' suggestion. I would like to see a design for a homemade Parr reactor. Something that could be used for high pressure and high temperature reactions. Possibly even equipped with a temperature indicator, pressure indicator, and mixer. The design could then be verified by making a useful reagent that's difficult to obtain.

Today on the History channel a scientist was attempting to simulate conditions at the bottom of the ocean near hydrothermal vents. He used a metal screwed cap cylinder placed in a tube furnace. Attained pressure was several hundred atmospheres.

Klute - 29-7-2008 at 18:30

Indeed, a hydrogeantion apparatus would be very usefull! But considering the hazard, i think that the construction of a some what low pressure vessel first might be safer, to be able to notice the potential problems, and how these would go with higher pressures. A bit like starting a small scale reaction before scaling up

Higher pressures means cheaper catalysts too

I wonder what things like Cu/SiO2 and Ni/C could do even at 3 atm, and if they could rival with expensive palladium and platinium...

Ah, i could do with such an apparatus right now, trying to mono-methylate that !@*ù#$ b-phenethylamine...

Ozone - 29-7-2008 at 20:07

Heck! I had not thought of that one, but a reliable home-brew hydrogenation apparatus would definitely be a winner.

I have wondered about using a bi-phasic system under pressure with H2 generation in-situ? I suppose you might need a flocculant to keep your catalyst where-you-want-it.

Cheers,

O3

kilowatt - 29-7-2008 at 20:33

Some moderate to high temperature syntheses would be good to see too, and I think they would go well with len1's skills (this is one of my favorite areas of chemistry). For example CaS, CaC2, SO3 from the Contact Process, SO2 from calcium sulfate reduction, elemental silicon from silica and carbon, etc. Some of these require electric arc or oxy-fuel temperatures, but those can definitely be done at home with a little ingenuity.

Another thing that comes to mind is boron trihalides from halogen and boron trioxide/carbon at moderate temperatures.

I'm not sure if this still falls under the category of reagents, but some low temperature stuff would be interesting too, and I don't recall ever seeing a home chemist do it. I have always wanted to make a simple sterling or pulse-tube cryo-refrigerator (it does not seem outside the amateur scope at all, using modified compressors or lawnmower engines) for liquefying nitrogen, oxygen, natural gas, crystallizing dry ice, etc.

Magpie - 31-7-2008 at 11:36

Len, I remembered an old thread that is related to your question. If you need any more ideas take a look at:

http://sciencemadness.org/talk/viewthread.php?tid=1359&p...

[Edited on 31-7-2008 by Magpie]

Formatik - 31-7-2008 at 14:27

N2H4, KNO2, CaC2, HCl (from a chloride and H2O at high temp), H2O2, CaO2, Al powder (from molten Al and steam), SnCl4.

kclo4 - 31-7-2008 at 14:53

Personally I think with len1's talent, making some of the simple molecules or ones that are easy to get would be waist of such talent, and the pictures wouldn't even be that important, but that is just what I think..

No offense, but KNO2, N2H4, and HCl are not really that hard to get or make. Making them in a complicated way isn't to helpful for the board, and since len1 is asking, I think he wants to be as useful as possible to the board, right?

Just In case you didn't know, Potassium Nitrite can be produced by grinding Potassium Nitrate and Carbon into a very fine powder in 2:1 molecular ratio and then heat until it ignites. I've done this reaction, and it seemed to work well, and if it needs to be pure, fractional crystallization probably wouldn't be all that hard at all.
2 KNO3 + C = 2 KNO2 + CO2

Do they make Al powder from molten Al and steam? That sounds very interesting but also kind of improbable... Seems to me that it would simply react with the Al and make Al2O3 and H2, and wouldn't you want it to be water not steam? I imagine you would inject water into molten Al and the heat would cause the water to flash boil and blow Al particles everywhere. - have a link about it?

Len1, have you decided on anything or do you still want more suggestions? Perhaps you could, when you get down to the top 10 or so chemicals, make a poll and have people vote for what ones to make first? - just an idea

I think more members should make illustrated guides, that would be great! especially for the Home Chemistry society
http://www.homechemistry.org/index.php?title=Main_Page

I'll make it a personal goal to make some sort of illustrated guide.. eventually when I get my new sink installed and get the scale, as well as a few chemicals that are coming.

Formatik - 31-7-2008 at 16:39

Quote:

Originally posted by kclo4
Personally I think with len1's talent, making some of the simple molecules or ones that are easy to get would be waist of such talent, and the pictures wouldn't even be that important, but that is just what I think..

No, they're not hard to get. But availability misses the point and fun of the chemistry. To add to that, availability comes and goes.

Quote:

Just In case you didn't know, Potassium Nitrite can be produced by grinding Potassium Nitrate and Carbon into a very fine powder in 2:1 molecular ratio and then heat until it ignites. I've done this reaction, and it seemed to work well, and if it needs to be pure, fractional crystallization probably wouldn't be all that hard at all.
2 KNO3 + C = 2 KNO2 + CO2

How were you able confirm nitrite formation?

Quote:

Do they make Al powder from molten Al and steam? That sounds very interesting but also kind of improbable... Seems to me that it would simply react with the Al and make Al2O3 and H2, and wouldn't you want it to be water not steam? I imagine you would inject water into molten Al and the heat would cause the water to flash boil and blow Al particles everywhere. - have a link about it?

Water vapor or air is blown into molten aluminium and aluminium dust forms. The product is usually dark grey and looks almost like zinc dust (Gmelin Al [A] 165). The original reference is Aluminium Bronze Powder and Aluminium Paint, New York 1927, J.D. Edwards.

kilowatt - 31-7-2008 at 17:36

Why not just melt aluminum and force it through a small orifice to atomize it? It could be atomized and collected under an inert atmosphere. An electrostatic charge between the collection vessel walls and the orifice could help it atomize.

[Edited on 31-7-2008 by kilowatt]

len1 - 1-8-2008 at 01:09

Thanks once again for the very interesting suggestions. I particularly like something that has an industrial chemistry bent to it. Plus with a bit of uncertainty in the result to make it an adventure. Although sometimes what seems like a tried and tested procedure can turn out to be a fizzer - Vogels hydrolysis to benzaldehyde to wit.

Of the things I hadnt thought off I liked the idea of hydrogenations and transition metal catalysts - but ill have to figure out what to make with that.

I also liked LiAlH4, but on checking the local Sigma-Aldrich stockist theyve plenty in stock and I couldnt find anywhere the word restricted. A concern though is the price $500/500gms for a piddly 95% grade, and it doesnt get cheaper with quantity. I wonder if it that might make it worth synthesising - even proper labs might have trouble running a research program with that price. What do people think?

I have just stumbled on one that Im even better prepared to synthesise - K, theres none in the country according so Sigma, it has to be brought in from the States at a cost of $117/50gms for 98%. Theres also this - Castner makes no claim to K for his cell, why? Is that because he didnt see why anyone would be interested in 1891, or does K dissolve much better than Na in the caustic bath so theres not even the narrow temperature window - I guess thats the element of adventure.

[Edited on 1-8-2008 by len1]

497 - 1-8-2008 at 02:53

Personally I would most like to see 1,2 Butylene Oxide. Another big one is DCM. While you're at it THF would be good

Ferrocene or carboranes would be formidable challenges and very interesting.

Practical fluorine would be a very impressive feat IMO.

Phosphorus would be awesome too. I might give it a try some time soon if circumstances permit.

Butyl Diglyme would be extremely useful for metal refiners.

Affordable Nafion style fluoropolymers would be interesting and very handy for many things electrochemical.

Nitronium tetrafluoroborate would be very nice.

BTW I think what you are doing is really great, keep up the good work!

Ephoton - 1-8-2008 at 02:56

yep im with K nice one. make it real pure please.

not_important - 1-8-2008 at 07:09

Len, potassium has been made with a Castner cell, as has NaK alloy. It is more soluble in KOH, less energy efficient and more bothersome because of that, but likely to be practical on a small scale. The greater reactivity of potassium can be troublesome.

Klute - 1-8-2008 at 09:53

Quote:

even proper labs might have trouble running a research program with that price. What do people think?

Never underestimate how wastefull a research lab can be

Once you see all that can be thrown away, all the purest/most expensive reagents used while ordinary grade would be more than enough... A friend of mine told me he was asked to get all the solvents and reagents in max. purity from the most expensive distributors, even though there where not needed, because it would be descrediting in the experimental otherwise

So the costs where easily doubled just to say "All solvents used where of purest grade bought from ****", even for column chromatography.......

I'll stop rating there

Ritter - 1-8-2008 at 10:22

Quote:

Originally posted by 497
Ferrocene would be formidable challenges and very interesting.

Even more interesting would be cobaltocene. It's red & pyrophoric!

I am personally interested in polyphosphoric acid from orthophosphoric acid. I think it can be done with a lot of heat in a heavy-duty metal retort. Basically you would be cooking it to drive off water.

[Edited on 1-8-2008 by Ritter]

len1 - 1-8-2008 at 10:29

Quote:

Originally posted by Ephoton
yep im with K nice one. make it real pure please.

Ill do my best. How about kosher? Call it Kosher-K. No seriously while searching their catalogue for pyridine (someone mentioned) I found they stock it in Kosher grade!??

Not_important, you dont by chance remember where youve seen that? It would be useful.

Klute, and I thought I worked in such a govt physics lab. Its better than your friends story - people dont just buy expensive stuff when cheaper would do, theybuy it when they dont need it at all. What the hack its taxpayers money. Ah but recently the cows started to come home - having wasted millions they might not be able to afford wipes any more - I suggested we might even have to bring our own toilet paper ..

Nicodem - 1-8-2008 at 10:48

Currently I have no reagent to propose, at least no inorganic one. As far as organic reagents go, I think an illustrated preparation of some sulfonyl chloride like TsCl, MsCl, EtSO2Cl, etc. would be great, especially considering how useful these are. Admittedly these reagents, as far as I know, can also be bought from chemical suppliers without troubles, but I thought they would fit Len's tradition of sulfur and chlorination chemistry. Also, more or less all the needed literature is already supplied on the forum.

[Edited on 1/8/2008 by Nicodem]

The_Davster - 1-8-2008 at 10:59

I am not proposing a product, but a methodology.

Start from, dirt, rocks, minerals, plant extracts and other naturally occuring materials and see how many transformations you can do using only naturally occuring things to end up with something really unexpected given the starting materials!

Start at the real ground floor of chemistry!

I plan to do this sometime, but I need more space first.

497 - 1-8-2008 at 11:00

Aww come on! Just plain old potassium???

Really that would be quite interesting. What do you people need it for?

Quote:

polyphosphoric acid from orthophosphoric acid

AFAIK the only way do go is heat the crap out of it in a copper crucible. I suppose it could be dehydrated by something like B2O3, but I don't see the point in that.

woelen - 1-8-2008 at 11:16

A second thing comes to my mind. It would be nice if acyl chlorides would become available for more persons, but inorganic stuff like thionyl chloride, sulphuryl chloride and phosphoryl chloride would be very nice as well. In many countries these are VERY hard to obtain and having a method available for synthesizing such chemicals at home would be great.

Ritter - 1-8-2008 at 11:48

Quote:

Originally posted by 497

Quote:

polyphosphoric acid from orthophosphoric acid

AFAIK the only way do go is heat the crap out of it in a copper crucible. I suppose it could be dehydrated by something like B2O3, but I don't see the point in that.

I want to be able to recycle it rather than disposing of it & buying new PPA. That way sounds expensive & wasteful.

[Edited on 1-8-2008 by Ritter]

kclo4 - 1-8-2008 at 13:10

Quote:

Originally posted by Schockwave

How were you able confirm nitrite formation?

I added Conc. Hydrochloric acid to my Potassium nitrite and a large amount of NOx was produced, and that would never happen with Potassium Nitrate. I don't know how pure my Potassium nitrite is since i have never attempted to figure it out, but it seems to be pretty pure.

Zirconia

chloric1 - 1-8-2008 at 14:19

Kirk's work talks how zirconium silicate can be processed with either sodium carbonate or hydroxide to leave free zirconia (aka Zirconium dioxide). As most pottery sources generally only sell zircopax or zirconium silicate, and lye fusion followed by hydrolysis in water would be quite interesting. Especially since the hobbyst only needs to perform a chlorate boosted thermite to get zirconium metal to add to his element collection.

kilowatt - 1-8-2008 at 14:57

What about some CVD? Pyrolytic boron nitride, metals and alloys, metal oxides like alumina and zirconia, even pyrolytic graphite. These require gaseous reagents in the proper ratios at low pressure and moderate to extreme temperatures.

DJF90 - 1-8-2008 at 16:02

Here's a proposition:
- Find a good method of making thionyl chloride
- Use the thionyl chloride to make anhydrous AlCl3
- Find a good method of making NaH
- React NaH with Lithium salt => LiH
- Find a way to purify LiH
- Use LiH and AlCl3 to make LiAlH4
- Purify the crude LiAlH4

Also, other interesting thoughs are:
- P2O5 from phosphates/other common phosphorus bearning stuff? And then use to dry reagents/produce SO3/N2O5

- Acetic anhydride via Sulphur chloride (I cant remember which chloride, it's been mentioned on SMDB before though)
- Diborane and it's use as a reducing agent; advantages/disadvantages/limitations
- Phosphorus... Once we have a method of producing the white allotrope, maybe you can extend your studies and find the best method of converting this into the red kind

much nicer stuff to work with

Klute - 1-8-2008 at 16:45

I'm getting fairly intereste din diborane too, but there isn't much to it experimentally speaking, it can be generated from NaBH4 with lots of reagents: BF3, AlCl3, I2, TFA, H2SO4, etc

I guess Len is looking for a litttle more challenge

DJF90 - 1-8-2008 at 16:55

P2O5 is definately useful in the lab

and fairly hard to get hold of

but getting a decent amount from a viable method other than burning elemental phosphorus ought to be a decent enough challenge

Formatik - 2-8-2008 at 15:08

Quote:

Originally posted by kclo4 I added Conc. Hydrochloric acid to my Potassium nitrite and a large amount of NOx was produced, and that would never happen with Potassium Nitrate. I don't know how pure my Potassium nitrite is since i have never attempted to figure it out, but it seems to be pretty pure.

Great then it's another possible way to get nitrite. But the reaction does not always go as theoreticized, and it's possible to end up with side products like K2CO3, K2O, etc. I also know too much carbon will get KCN (Polverone has done some experiments with this).

ScienceSquirrel - 2-8-2008 at 15:30

Triethylborane

The fabled green flame, inflames on contact with oxygen and poisoning by trace amounts results in auditory hallucinations.

Only kidding :-D

kilowatt - 2-8-2008 at 16:58

Triethylborane is just made via a grignard reaction, quite interesting though, I'd like to try it someday when I have a suitable setup and the time and guts to do it. Speaking of borane fuels, I have a complete synthesis for pentaborane that I got from a pdf of some medical journal. It can be found here on page 15. http://www.idecefyn.com.ar/mmcv08/O1.pdf Oh yes, and Triethylborane is quite innocuous when compared to pentaborane.

[Edited on 2-8-2008 by kilowatt]

ScienceSquirrel - 2-8-2008 at 18:26

I am kidding about triethylborane, I cannot see it as a home chemistry target.

If you want to die in a hurry, try messing about with stibnite, readily available down your local rock shop and you can make all sorts of antimony compounds from it with ease.
Boiling with zinc powder and hydrochloric acid is particularly recommended.
Acute stibine poisoning is slow, agonisingly painful but inevitably deadly at quite low doses.

[Edited on 3-8-2008 by ScienceSquirrel]

len1 - 9-8-2008 at 19:41

Thank you everyone for the suggestions. I decided to start with the following

1) potassium via castner
2) SOCl2 - this has already been started but needs improvement
3) LiAlH4

They wore chosen because they present an opportunity for original research (with none particularly well researched for lab synth) and because their synthesis might present an interest for research labs as well due to price/restrictions/haz chem (I want to shift the emphasis in what I do slightly towards the professional realm partly because there are not many people doing amateur chemistry, partly because one has to move on)

[Edited on 10-8-2008 by len1]

Panache - 27-8-2008 at 00:08

What about a benchtop micro NH3 plant using the Haber process. Or maybe a small fusion generator, supplying both helium and power to the lab.
btw those suggestions were simply compliments to your ingenuity not serious suggestions, however if you have any ideas.....

benzylchloride1 - 28-8-2008 at 17:30

The synthesis of O-Phenylenediamine from a phthalate ester via ammonolysis and a duble Hoffman reaction would be a useful synthesis. O-phenylenediamine would be useful for synthesisizing many useful heterocycles and ligands for use in inorganic chemistry. I am currently working on this synthesis, but the ammonolysis is taking some time.

Sauron - 28-8-2008 at 22:09

Well, o-phenylenediamine, once you have it, is very easily oxidized and so presents problems in purification, handline and storage.

Normally it is prepared starting from aniline, by blocking the 4-position via sulphonation, then nitrating selectively at the 2-position. Removing the sulphonic acid group at 4 position leaves o-nitroaniline. This is readily reduced to o-phenylenediamine. See Org.Syn.

BTW, I have a Kg of Merck o-phenylenediamine and they store it in dark bottles wrapped in opaque black plastic, because it is light sensitive.

It is also a nasty hepatotoxin, more so than aniline.

some belated organic ideas

Formatik - 29-8-2008 at 13:39

The synthesis of sulfoxides (DMSO, DESO, etc), or furfural (I know of the OrgSyn synthesis, but seeing it demonstrated is another thing).

benzylchloride1 - 31-8-2008 at 10:07

Another idea would be the synthesis of mono nitro toluene isomers and the separation of the isomers along with the production of the respective toluidines.

Panache - 1-9-2008 at 02:57

actually a serious request would be BF3 in ether, now that would be great!!!

Klute - 1-9-2008 at 07:37

I think BBr3 might be easier to form than BF3? Although they don't have the same properties IIRC.

OMG - 5-9-2008 at 12:21

I think the best payoff would be to put effort into finding a good way to produce ozone. If ozone could be easily produced with enough speed, then it would make chemical acquisition a lot easier IMO.

kilowatt - 5-9-2008 at 12:53

I second that. In theory ozone is one of the most amazing and versatile synthesis agents. Nitric and sulfuric acids and their anhydrides in particular come to mind. However I remain skeptical that it could be produced cheaply in enough molar quantity to be useful in any such syntheses.