Author Topic: Chloroform  (Read 263 times)

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Chloroform
« Reply #20 on: April 11, 2009, 07:21:39 PM »
There is something there but not much of it. Just some powdery looking stuff on the bottom. Probably trace amounts of chloroforms or something. I think my NaOH solution was alot less concentrated as I figured because the liquid was green/yellow from chlorine so tonight im going to boil it solid and go from there with the weight.

Another possible reason for it failing could be because it was two concentrated. The acetone sat on top and never intermingled so there is a little work to do in finding the best way. When I added extra water is when the little bit of stuff fell out.

Making a concentrated mixture of NaOCl then slowly dripping one into the other so there is excess seems like it would be the best means.


Any suggestions on which one to drip?
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Chloroform
« Reply #21 on: April 11, 2009, 07:25:53 PM »
Honestly I'd just go by the strongest bleach solution you can find in the store and then add acetone. To much acetone will react with the chloroform and I think it will form chlorobutanol so drip the acetone into the bleach solution.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Chloroform
« Reply #22 on: April 11, 2009, 07:32:23 PM »
Ohhhh Chlorobutanol Eh....

Well thats probably whats chillin on the bottom then.

Chlorobutanol
Appearance White solid
Melting point 95 - 99°C
 
Ok atlest note alls lost. I got some hypnotics to test. Any know know of the dosage of Chlorobutanol?
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Chloroform
« Reply #23 on: April 11, 2009, 08:09:27 PM »
considering you only might have accidentally made chlorobutanol with an untested method, I wouldn't go about trying it!
You could get something that is over chlorinated or chlorinated in the wrong places that could be one hell of a liver toxin. I think chlorobutanol is a pretty good liver killer as is.
I'd just make some chloroform the normal way with bleach, and then do base catalyzed reaction with acetone to get some nice pure chlorobutanol with a crystallization at the end for something like that.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Douchermann

  • Dominant Queen
  • ****
  • Posts: 397
Re: Chloroform
« Reply #24 on: April 12, 2009, 09:23:31 PM »
I think acetone is turned into the enolate in the presence of NaOH, but I could be wrong.  Either way, produce the NaOCl first (remember, 30% is about the highest you can go at STP), then mix the acetone.

As for chlorobutanol, I would recommend 1.5 to 2g for some fun.  My buddy tried it at 2g and says it makes him extremely drunk feeling for about 2-3 hours (usually the longest you can stay awake) but then you pass out for ridiculous amounts of time.  He slept 27 hours I believe it was.  Relaxation can be had from 300mg and sleep induced from 1g.  Don't try this stuff though, there is far too much going on in that reaction.  If you wish, just make it from the chloroform you produce - it doesn't take much to make quite a bit.

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Chloroform
« Reply #25 on: April 12, 2009, 09:27:18 PM »
Wouldn't 2 grams of chlorobutanol pretty much destroy your liver?
If you are playing with chlorine gas, you could just mix that with anhydrous ethanol and do a few other things to get some chloral hydrate. Everything needs to be really dry though, or it will fail.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Douchermann

  • Dominant Queen
  • ****
  • Posts: 397
Re: Chloroform
« Reply #26 on: April 12, 2009, 09:40:55 PM »
People binge drink all the time, which is so much worse on your liver.  They often follow this by loading up on tylenol (acetominophen) the following day to cure the hangover, which just puts more strain on an already overworked liver.  If you only use 2g once or twice, it wont hurt you too much.  2g of chlorobutanol would not form an addiction.  No one would be able to live a desirable life if they constantly sleep 24 hours.

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Chloroform
« Reply #27 on: April 13, 2009, 12:03:22 AM »
http://www.geocities.com/nepalorganic/wwh.htm?20095

Reactions 5 and 6 seem like a very good way to go for chloroform. Any one have experiance with bleaching powder?
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Chloroform
« Reply #28 on: April 13, 2009, 01:07:20 AM »
Interesting! Bleaching powder is calcium hypochlorite, I think most stores sell it as a pool chlorinated in the range of 40-50ish percent, the rest probably being calcium hydroxide and calcium chloride. I'd like to give a better percent but I cannot. I think it is perhaps 48% calcium hypochlorite?

That would be great if ethanol + bleaching powder worked out well.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Chloroform
« Reply #29 on: April 13, 2009, 02:48:35 AM »
It says it right on the package how much hypochlorite is in them its just the other stuff they dont speek of. Good part is they measure it W/W IIRC so doing the math for just the calcium hypochlorite should pose no problem and you will get a very concentrated amount of hypochlorite instead of 3%-5%. Ill give it a go soon maybe tonight with acetone(no ethanol :-[ sobar sedits bord) like they said but it seems to me that chloroacetone would be a problem so I think Im going to just lead the contents from the heated flask right into ice water.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Chloroform
« Reply #30 on: April 13, 2009, 02:54:51 AM »
I highly doubt chloroacetone would form.. this is the same reaction as before though.  The beauty of using ethanol and bleaching powder in my opinion is it gets rid of the risk of any acetone reacting with the chloroform in the basic solution.
ethanol actually stabilizes chloroform.
I wonder why methanol or something like that wouldn't work? Think isopropyl alcohol could make some interesting halocarbons? That might be worth trying sometime - mostly likely produce chloroform since acetone does and they are basically the same, you'd just end up with different byproducts.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Chloroform
« Reply #31 on: April 13, 2009, 04:14:55 AM »
http://www.erowid.org/archive/rhodium/chemistry/chloroform.html

This seems more up my ally then using buckets of bleach and gallons of acetone.

This is what I want to try by chlorinating EtOH

Quote
When chlorine is passed into boiling alcohol, both chlorination of the methyl group and oxidation of the primary alcohol group to an aldehyde occur, giving trichloro-acetaldehyde or chloral: When chloral is treated with caustic alkali, fission of the C-C linkage occurs, giving chloroform and a formate. Acetaldehyde and also many ketones, such as acetone, containing the CH3CO- group behave similarly when treated with calcium or sodium hypochlorite, chlorination of the CH3CO- group being immediately followed by fission of the molecule by the alkali present in the hypochlorite solution. The acetone method clearly gives a much cheaper product than the alcohol method.

So we feed chlorine into warmed EtOH until the correct weight has been gained then hydrolysis with NaOH. Products will be two useful materials Chloroform and sodium formate which can be made into formic acid when needed. This seems way more cost effective then the other methods using dilute bleach solutions. They say the acetone method give a cheaper product but i dont know if they are talking about quality or cost effectiveness. Either way I feel that EtOH should produce a much cleaner and higher yeilding result without using buckets full of stuff that needs to be chilled.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Chloroform
« Reply #32 on: April 13, 2009, 04:25:54 AM »
Chloral is a bit tricky to make as everything needs to be totally dry. Very dry chlorine, absolute ethanol, and so on. You're just making chloral hydrate with out the hydration step at the end.

Quote
This seems more up my ally then using buckets of bleach and gallons of acetone.

Its only a tiny bit of acetone! I, having failed the bleaching powder method (run-away) and a few other methods, really prefer the gallons of bleach + some acetone.
I did it in a 5 gallon bucket in the winter when my bleach were full of ice crystals and got great yields, and it was easy to separate. I separated it after letting it sit for a while to get all the chloroform in the bottom, and then just poured most of the water off into another bucket, I sucked the chloroform up with a turkey baster and then refined it a bit more.

To each is own, but I'd give the bleach + acetone a chance.
I guess I just don't think the bleaching powder works well since I've had problems with it. You could get tons better yields then me, and hopefully you will.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Chloroform
« Reply #33 on: April 13, 2009, 04:47:36 AM »
I hope I do to
I like chlorinated solvents above all else. They rip the fuck out of anything but yet can be used selectively also as long as you got the correct one. Best of all.....Nooo Fires. And when you go getto fires are always at the top of your mind because they can end a nice peaceful life of freedom.Im going to screw around with differnt ways and let yall know whats best... who knows it may just be the buckets of liquid.
Wish me luck.

Dryness should be no problem for me Iv been a dry freak sence I started Org chem because one of the first things I read was about how powerful a catalyst H+ -OH is. That an Iron can fuck up your whole day quicker then shit.
« Last Edit: April 13, 2009, 04:50:18 AM by sedit »
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Chloroform
« Reply #34 on: April 13, 2009, 04:51:23 AM »
Will do!  :D If you find a better way I'd love to try it as well, so make sure you take notes!  ;)
I've been needing some more chloroform.. I can't remember why, but I do.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Chloroform
« Reply #35 on: April 13, 2009, 05:12:51 AM »
LOL honestly I have about a half liter of it but its about 40-45 years old atlest so opening it isn't on the top of my list. My grandfather use to have a darkroom so he has a stash of great chemicals around that they dont let me near to much because they had to lock household chems up when I was like.. 11. Hes old now and Im alot older. If i want them there all mine, no doubt. But using 50 year old chems scares the shit out of me a little.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Chloroform
« Reply #36 on: April 13, 2009, 05:18:42 AM »
old chloroform - I assume the fear is phosgene? I'd add some urea, and some ethanol/methanol (possibly dissolve the urea in the alcohol?) and that should clear any phosgene up.

Age would only bother me depending on the chemicals. Old potassium nitrate might as well be as good as new.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Chloroform
« Reply #37 on: April 13, 2009, 06:35:07 AM »
Little bit a fear of phosgene, but since its Kodak which is commercial chemicals I dont think they would let it slip without stabilizers and such...but this is also many moons ago so god knows there standards. I leave his chemicals alone for the most part because I feel they may have sentimental value to them for him. his son died at 16 and that was there hobby so until "that" time comes ill leave them be because there not worth the remorse of just taking them.... ask for them and I could have them but I dont feel the need to. I enjoy making all my own chems from basic things. When the DEA locks down table salt I will still be having fun. Iv always been a chemist before a user so its all fine for me.

There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Chloroform
« Reply #38 on: April 13, 2009, 06:49:36 AM »
Ah I understand where you're coming from. I'm an ALL OTC person for the most part but organic chemistry gets a little impossibly with OTC materials. Damn good luck making modafinil OTC lol (..other then probably from diphenhydramine, which I never considered at the time) I've really only got H2SO4, KMnO4, Sulfur, and Oxalic acid from a chem supply, but that is when I was a bit younger.
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Chloroform
« Reply #39 on: April 14, 2009, 02:51:26 AM »
I made some sort of chlorinated solvent today but I cant confirm its chloroform until its distilled and a BP test is done. Acetone was mixed with 47% damp bleaching powder. A few drops of HCl was added causing a large release of Cl2 into the acetone. There was some heat generated but it was a small scale so very controlable with a cold water bath. This was allowed to react for about an hour or two and then the yellow acetone was decanted off into another container. NaOH solution was added and the whole mixture turned deap purple/red color(This could be due to trace nickle/copper chloride contamination but I dont know) and opaque. This was left to set for a little while and the mixture turned more of a yellow orange with a thick fluffy layer at the bottom... Well it filled almost the entire amount of fluid so we will say there was a thin clear layer at the top. After droping this in H2O it was clear this is some form of denser solvent because it formed beads and droped streight to the bottom. It has a sweet scent to it unlike acetone or chlorine but more like a sweet mixture of both. I feel that the chlorine in solution never really chlorinated much of anything and the addition of the NaOH formed a very concentrated form of NaOCl creating chloroform. This is all just speculation at the moment until its distilled and a BP test is performed to see which chlorinated solvent formed.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!