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Author: Subject: Experimental Preparation of Chlorobutanol
Madog
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[*] posted on 24-1-2004 at 22:32
Experimental Preparation of Chlorobutanol


Chlorobutanol is a seditive, knockout type drug. In the body it yields the same chemical that causes the effects of chloral hydrate, a comercial sleep aid. So their effects are identical. Today i made some chlorobutanol, for no reason specificaly.

First i had to prepare chloroform.
750ml bleech were added to a 1000ml beaker with some crushed ice, it was let to cool and agitated a bit. 15ml of acetone was added to this and it was stirred wit ha stirring rod. I like it sit for about a half hour and it clouded up alot, i stirred it more, let sit, stir, until it had cleared up mostly and there was a bunch of clear non-polar liquid at the bottom. 600ml of the waste was decanted. the rest put into a sep funnel and the chloroform dripped off.
yield: 10ml

the 10ml chloroform, 90ml acetone and 2g NaOH were mixed together in a beaker and set in the freezer for 2h 30 minutes with occasional swirling. the solution clouded up to the point of opacity after the first few minutes. that was filtered to remove the NaOH and most of the excess acetone was distilled off(just a little left). the opaque yellowish liquid left over was poured into cold water and stirred, the liquid at first sank to the bottom then with stiring they formed crystals.

these were filtered and the filter suspended over CaCl2 in a beaker, it looked like the paper got a small rip and some leaked through onto the deciscant, but it may have jsut been water dripping that was forsome reason yellow, or maybe some actualy melted in the warm room. but in the end, the semi-dry yield was 4g. it had some moisture left. 6 capsules were filled with this, each one cointaining 600-800mg of the semi-dry product.

i dont know when i'll get around to testing it on myself, not tonight, and im not especialy keen on doing it on a schll night, and this comming weekend i may not be able to do it. but i will post about it when i do.

[Edited on 1/25/04 by Madog]

[Edited on 1/25/04 by Madog]




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[*] posted on 24-1-2004 at 22:39


nooo! argh! i didnt notice an identical thread half way down the page...



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[*] posted on 26-1-2004 at 10:12


I too have done experiments with chlorobutanol lately.

My chloroform was prepared from 700ml 6.25% bleach, and 15 ml of acetone. This yeilded 8ml of chloroform.

72 ml of acetone was added to a 250ml beaker and 1.6 g of NaOH was stirred in. There was not a complete dissovation of the hydroxide, and some remained at the bottom after quite a bit of agitation. Then, the 8ml of chloroform was added in three parts and stirred. Almost immediately after addition, the mix turned cloudy. Stirring was done with the end of a zip tie, which is quite convenient.

The mix was placed in the freezer and stirred whenever I thought about it for around two hours. There was still a small amount of NaOH solid on the bottom. I poured this through the filter paper, and as it was going down, it reminded me quite like milk. The filter was discarded and the filtrate put on the lowest setting of a hotplate. I left and came back 30 or so minutes while the acetone heated off. I came back and there was a slightly yellowish liquid sitting in the beaker bubbling slightly, which I predict lost a good amount of product.

The liquid was quickly poured into a beaker of cold water, me not wanting to lost any more product. At first, I was dissappointed due to the lack of crystals or PPT, but after 15 seconds or so of stirring, fluffy crystals started to form. The circular motion of my stirring formed a 'cone' of the crystals in the middle of the beaker, around 2.5 cm high and a a bit wider. Hurray! I probably thought. The crystals were fluffy and reminded me of wax. They were filtered out, washed with cold water, then filtered again.

The odor was something I have not smelt before, so I assume that is what camphor smells like. It is strong, but slightly sweet, with a slight hint of something like licorice. The wet crystals stick together, so I mashed them out on the filter paper so they could dry better.

According to calculations and Madog's results, I should get around 3.2 grams, however it is still wet and I have to wait.

[Edited on 26-1-2004 by Haggis]




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[*] posted on 26-1-2004 at 15:58


mine is reverting back t the liquid in the caps.

a while ago i had made it, and for some reason, i dont remeber, i didnt put it in water, and just put it in a vial. i put this in the freezer to see if it would freeze, it never froze, still have the vial of it, anyone have an explanation for its behavior in changeing states?




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[*] posted on 26-1-2004 at 19:53
IMPURE


IMPURE

its not pure. One of the concrete definitions of a pure substance is a sharp freezing/melting/boiling point.

Pure chlorobutanol is a dry colourless/white crystal.

Look on page 100/101 of James Zubricks organic lab survival manual. It will give you detailed instructions for recrystillization. Chlorobutanol will probably best be served by a mixed solvent recrys. etoh/h2o.

Then followed by a sublimation (pyrex pot with dry ice in the center of the inverted lid and slow application of heat on the bottom should prompt crystal growth on the glass knob).

I would not skip the recrystillization step though. The mixed solvent system will most likely lead to an oiling out of your chlorobutanol. Don't worry, its common with mixed solvent systems.

There were some instructions on recrystillization on another part ot this site but were somewhat innacurate.

If you don't have James Zubricks little manual, buy one! it is the best 20 bucks you'll ever spend. Buy it before anything else. It is written in plain english for the average first year student.


It's helped me immeasurably. :D

[Edited on 28-1-2004 by Hermes_Trismegistus]




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[*] posted on 26-1-2004 at 20:05


I think madog and all of us who have been here a long time are used to the edit button never working for a year or so.



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[*] posted on 27-1-2004 at 12:13


Yea, if memory serves correct, it was about a year ago around this time when the edit function kicked on. Oh well.

After washing my chlorobutanol well, I figured it was time for a slight taste test. I was marveling at not worrying about neutralization and how sensitive this white powder I was filtering was, I am used to other compounds.

I took .02 grams of the chlorobutanol. Then I licked my fingers, and found a strong, chemical, astringent taste. It was pasty on my toungue and roof of my mouth as I did the 'tasting' motion. Soon after, that area of my toungue went slightly numb, attributing to the topical anestetic properites. The chemical flavor was persistant and was dispatched with a few swigs of orange Gatorade.

On a usual night for me, I dream throughout the night, waking up often. I went to bed normally, but when I woke up, I found that the beginning portion of the night seemed to be oddly missing. As if I had forgotten about it, it felt empty.

I really should not be consuming such things, and I appologize to my kidneys. This was just preliminary testing, perhaps I shall do more in depth tests sometime soon. I'll see what else of the properties of chlorobutanol I can whip up for my fellow mad scientists.

Update: my chlorobutanol does not produce a change in pH paper. This can mean that it is close to neutral, or it could also mean that somehow my micro sample didn't register enough to produce a change.

[Edited on 28-1-2004 by Haggis]




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[*] posted on 27-1-2004 at 16:13
Wow Haggis. Your crystals were white huh!??


You do seem to have gotten a greater purity than others have(see the original chlorobutanol thread for details)

And I am thinking that the reason may be the longer and more vigorous heating of the oil phase while boiling off the excess acetone. Perhaps the contaminants are even more easily sublimated/vapourized than the chlorobutanol.

Only one way to find out. Fractional distillation to decomposition with either a large amount of product or a microscale kit.




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[*] posted on 29-1-2004 at 19:10


It ended up to be an exact 2 gram yield. The product was powdered with the flat end of a hot melt gluestick and introduced to a plastic vial, which I sealed tightly. Seeing the ease, cheapness, and potential interesting-ness of this chemical, perhaps I shall and try to produce larger batch quantities. Updates ahead.



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mad.gif posted on 29-1-2004 at 22:20
AAAARRRRRGGGHHHHH!!!!


After attempting this synth I suddenly am simultaneously frustrated and enlightened.

The other chlorobutanol thread shows a common occurence. Getting a discoloured and perniciously uncrystalisable substance yellow substance and getting a pure white product using sloppy methodology.

SWIM used to make herbal extracts when he was alot younger. Alot of herbal extracts and thus had ample opportunity to explore different OTC solvents.

A bane of his existance was this one type of rust inhibitor that he couldn't seem to separate from the various solvents he used, Even by distillation.

but for some reason when he finished his oily herbal extracts instead of boiling off with the sovent as it had done in prior solvent purification attempts, this damned rust inhibitor would remain in the oily emulsion that was so precious to SWIM's employers.

No-one ever knew about this damn rust inhibitor except SWIM. SWIM knew but since the customers loved the resinous extract and didn't seem to notice it, and the employers seemed to love the wonderful texture and smell the rust inhibitor gave to the oily product (as well as increased yeilds). SWIM never told anyone.

But the damn thing still pisses him off to this day.

and then SWIM synths "chlorobutanol" and while the excess of acetone is boiling off he smells something.

A chemically smell with definite earthy undertones. Normally no-one would identify it. But SWIM does. CUZ SWIM has smelled it before.

Its that damn rust inhibitor. THey put it into the metal cans of acetone, and when madscientists use the acetone to make chloroform it seperates into the chloroform and when those madscientists use an excess of acetone with the chloroform to make the chlorobutanol the damn inhibitor in the acetone gets sucked into the damn chloroform before it reacts and then just sits around in solution waiting to be concentrated by evaporation.

I can smell the camphorus odor of the expected chlorobutanol. But behind it I can also smell that damned earthy rust inhibitor.

PISS ME OFF :mad::mad::mad::mad::mad::mad::mad::mad::mad::mad::mad::mad::mad::mad::mad::mad::mad::mad:

to be continued..........




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[*] posted on 31-1-2004 at 10:27


At 12:00 midnight one evening I weighed out .3g of chlorobutanol into a film canister. Lime gatorade was poured into the canister and the 'shot' was taken. A bit of chlorobutanol was left on the bottom, so I took another one till it was gone.

The flavor was strong and slightly unpleasant, so I drank some more gatorade to dispatch the flavor. Then I sat down and read. After 25 minutes I started feeling 'slow'. I put down my book and layed down.

Then I don't remember much untill waking up around 5 am from a dream. I assume that the minimal amount of CB wore off from my system after around 4 hours, and I started dreaming, then woke up from it after it was no longer holding me asleep.

I then fell easily back to sleep till 12:00. This makes me assume that the amount I took was not sufficient, for my metabolism, to keep me asleep for the entire night, but the remenants of it in my system were strong enough to encourage me to sleep after the full effects wore off.

I won't have a good opportunity to test it's effects again for a while, unless I do it tonight. Note to self: find some empty gel capsules and fill them, the flavor isn't cool.




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[*] posted on 21-2-2004 at 17:39


I recently tried this reaction and I got...uh..interesting results. The first time I tried this I used exactly Haggis' procedure, and I got a yellowish product which reverted to the liquid within a week. the second time I tried the reaction I got a pure white precipitate. :cool: I used exactly haggis' numbers-but not the same procedure. After it was sitting in the ice bath for 2h I filtered it and after the filtering, the filtrate went from milky to yellowish( I dont know why this happened). I put the filtrate into a 125mL erlenmeyer flask, stoppered it, and put it back into the ice bath overnight because I was too tired to finish the procedure that night. The next day the yellow color was mostly gone, it was just very pale yellow. I did not bother with heating off the excess acetone, I just dumped the mix into cold distilled water. After filtering it was pure white. :cool:. And when I touched a very small ammount of it, my finger felt like it fell asleep.:o No results on yield yet as it is still drying.
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[*] posted on 29-3-2004 at 18:53


thats interesting. I'm going to probaly try this again sometime, i'll have to try waht you did.

my capsules with the material half reverted to the oil but styed at that. i still have them. never got around to performing a bioassay.




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[*] posted on 29-3-2004 at 20:40


Note: dont air dry it, most of mine evaporated, and dont dry it over drano, turns green. I really got to get a desicator.
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[*] posted on 30-3-2004 at 11:35


Yea, air drying results in loss of the product in substantial amounts. Rogue chemist you don't need to buy a dessicator. Just make one, it is extremely cheap and useful. If you want some info on building one just open a thread or U2U me.
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[*] posted on 30-3-2004 at 11:54


Explosivo, first result when I googled "improvised desicator" was on this site, one question though, is road salt(CaCl2 and NaCl) fine to use as is as a desiccant or should it be heated to drive off the moisture?
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[*] posted on 30-3-2004 at 11:57


I personally use home-made CaCl2 mixed with CuSO4. The mixture is heated strongly to remove the water of hydration. I guess this should also work for road salt.


[Edited on 30-3-2004 by Esplosivo]
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[*] posted on 30-3-2004 at 12:40


I bought a big jug of CaCl<sub>2</sub> sold for deicing ("Driveway Heat";). Should work fine, but to ensure freshness you can heat it on the stove. When heated in a metal pan, mine gives off very little water, unlike the masses given off by epsom salts. I used it to dry some Iodine crystals; it worked well (takes some time, though), but I think that was the stuff that I had processed on the stove.
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[*] posted on 30-3-2004 at 13:27


The CaCl2 sold around here for icemelting is covered in a layer of something. I think it may be CaCO3. If this is the same stuff others can procure, it's helpful to crush the prills a bit. The desication time is greatly reduced for me.
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[*] posted on 26-4-2004 at 11:26
In the pursuit of anhydrous chlorobutanol.


After reading the msds of chlorobutanol (1,1,1 trichloro 2 methyl 2 propanol) It was noticed that most pharmacopeia's list the hemi-hydrate form and only one or two list the anhydrous form.

so.......of course......monkey read.....

The recrystyllization of chlorobutanol has been difficult, the two solvents thats seemed logical to use acetone and xylene don't seem to work real well.

During evaporation of the chosen solvent the vast majority of the product seems to disappear. The scientist is not particularly proficient at chemistry and it took awhile for him to consider the possibility of the chlorobutanol forming an azetrope with the solvent and evaporating away together.

To Be continued....




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[*] posted on 26-4-2004 at 19:53


Interesting thread. I'm in the process of doing this as we speak! MUAHAHAH.

I found a good link:

http://www.monoxyde.org/chemistry/chlorobutanol.txt

Author recommends recrystallizing in ethanol, as it gives clean white crystals. Water can also be used, but from this guy's experience, he recommends ethanol.




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[*] posted on 27-4-2004 at 00:07


Well I'm finished...almost.

750 ml bleach (lemon scented - I had nothing else) with 15 ml acetone. I got about 4.5 ml (very shitty) of chloroform.

45 ml's of acetone was measured, added to a beaker. 1.00 g of NaOH added. Had a great difficulty dissolving it. It wouldn't all dissolve so I proceeded to add the chloroform. Turned milky instantly. Tried to get the NaOH to dissolve, a lot of trouble with this...Put it in the freezer for about two hours, stirring every 10-20 minutes (FINALLY got all the NaOH to dissolve after about 1.5 hours). After the two hours I removed it from the freezer, place it on a hot plate and let it boil.

When it was settling out, I noticed that the milkiness seemed to drop to the bottom while the acetone remained on top. I decanted the acetone/goods and placed it in a beaker. I then proceeded to boil both of them down (one had the milky stuff, the other had the decanted acetone/goods). The decanted one started to turn yellow after awhile. When I felt it was time, I removed both from the heat and added cold water to both. The milky one acted oddly, it became oilish in its structure and white stuff floated to the top. The decanted one dropped out crystals.

I filtered the decanted one and got some yellowish/orange crystals. Dried them up then decided to add more cold water to the milky one. What appeared to be the same crystals popped out from the oilly milk liquid. Filtered these crystals. This must be chlorobutanol, no?

Did a mixed solvent recrystalization with H2O/EtOH. I'm still waiting for crystals to come out, and it's not looking good. It didn't take much hot ethanol to dissolve all the crystals, about 5-10 ml's, and this was the minimum amount. Added some hot water until cloudy (about 1-2 ml's), then added more ethanol to clear it up. Let it sit at ambient temperature. Went out for a smoke, feeling pretty good. Came back inside, still no crystals. The solution is a yellowish/orange color, very camphory smelling (I love this smell...). I placed the flask in the fridge and still nothing. I guess I'll put it in the freezer but I doubt that will help. Hmmm. I guess the stuff is quite soluble in ethanol at room temperature then. But why would this author dude suggest to use ethanol to recrystallize? At the end of the article, someone else mentioned that they used 50% ethanol. I guess I may have to try that one...

Anyways, fun experiment. I finally have basically all my equipment, except my ohaus which I am patiently awaiting...I have a shitty digital that I used to mass everything..ugh. I got my stands today and this opened a whole new dimension. Very exciting.




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[*] posted on 27-4-2004 at 09:58


Quote:
Originally posted by thunderfvckAfter the two hours I removed it from the freezer, place it on a hot plate and let it boil.

I then proceeded to boil both of them down (one had the milky stuff, the other had the decanted acetone/goods). no?


Perhaps not, you applied alot of heat to a delicate reaction. Perhaps next time try to keep the reaction cold throughout. Use a vacuum to dessicate or just dry normally while maintaining cold temperatures.




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[*] posted on 27-4-2004 at 11:03


The reaction was kept cold until the boiling of acetone began. Even when I started heating it (at the lowest heat possible) the precipitate fell to the bottom. I think it was just a matter of letting it sit.

Anyways, after putting it in the freezer for like, 5 minutes, MASSIVE precipitate :D

I added some cold water to get it moving, filtered, pat-dried...Yield was 2.17 g. Slightly orange in color. I haven't taken a melting point yet (I will as soon as I get home...)...But I tried some on my tongue, NUMBNESS!! I'm so excited (and I just can't hide it! Oh no no no, I know I know I know I know I know I want you, I want you).

I think I'll recrystallize it again from cold ethanol (to hell with the mixed solvent), and see how that turns out.

I'll take some in time, in time...




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[*] posted on 27-4-2004 at 15:07
Oh I get it!


When you read the literature, you must have assumed that the "distillation" occured at above room temperature and at normal pressure.

And that's why everyone is boiling it.

I have a vacuum pump so I distil acetone at quite a low temperature.

When I didn't have a vacuum pump I did the reaction in the freezer and then used a whole bunch of plates to evaporate off the acetone.

I poured about two or three ml's onto a cool plate, swirled it around and put it to the side, then I would repeat with several more plates.

By the time I went back to the first plate, almost all the acetone would be evaporated.

The pure white crystalline slurry would then be recrystallized and washed with water.

Perhaps your boiling of the chlorobutanol/acetone mix was decomposing it into something else.

That would account for it becoming orange and oiling out.




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