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OfflineKonnrade
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Synthesizing Chloroform
    #5492012 - 04/08/06 05:47 AM (18 years, 1 month ago)

I present this more for an entertaining read than for anything else. Chloroform is good for nothing other than use as a solvent. It's recreational use has a nasty tendency to cause severe, life-shortening liver damage. Besides, most of the time exposure to chloroform merely causes unconsciousness.

Nonetheless, I find it interesting that chloroform can be synthesized from two chemicals that are found in most of the homes in america. You are very likely to posess them at this very moment!

Quote:

Required: Calcium Hypochlorite 100g (bleaching powder), acetone 44ml

Place 100g of calcium hypochlorite in a mortar and add 250 ml of water in small quantities at a time: between each addition grind the mixture of bleaching powder and water well together and decant the cream-like suspension through a funnel into a 1-litre flat-bottomed flask. Finally, when all the water has thus been used, only a gritty residue remains in the mortar. Fit the flask with an efficient reflux water-condenser, pour 44ml (35g) of acetone in small quantities, at a time, down the condenser and mix by thorough shaking after each addition. The reaction usually starts spontaneously after a few minutes, and a bath of cold water should be available into which the flask may be dipped if necessary to moderate the reaction. Should the reaction show no signs of starting within 5 minutes of the addition of the acetone, warm the flask cautiously on a boiling water-bath until the reaction starts, and then remove it immediately. When the vigorous boiling has subsided, heat the flask on a boiling water-bath for a further 5-10 minutes (not more) to complete the reaction. Cool the flask in cold water (to prevent loss of chloroform vapour whilst the apparatus is being rearranged) and then fit the flask with a fairly wide delivery-tube and reverse the water-condenser for distillation. Heat the flask on a water-bath until distillation of the chloroform is complete.

The chloroform thus obtained is usually acidic. Therefore shake it thoroughly with dilute sodium hydroxide solution in a separating-funnel. (If the chloroform tends to float on the alkaline solution, it still contains appreciable quantities of acetone: in this case the soda should be run out of the funnel and the chloroform shaken with water to extract the acetone. The extraction with the soda can then be performed after the water has been removed.) Carefully run off the heavy lower layer of chloroform into a small conical flask, dry it over calcium chloride for 15-20 minutes, and then filter it directly into a 75 ml. distilling-flask fitted with a clean dry water-condenser. Distill the chloroform, collecting the fraction of bp. 60-63�C. Yield, 30g. (20ml).

Chloroform is a colourless liquid, of bp 61� and d 1.50. It has a characteristic sweetish smell, and is frequently used as a solvent in organic chemistry.




That details a synthesis of chloroform by means of mixing acetone and hypochlorite. What is hypochlorite, you ask? It's the active ingredient in the bleach that you have in your laundry room.

Of course, synthesizing with household chemicals is hazardous. Especially when the reaction is very exothermic.

If one were to do this at home, which isn't a very good idea, they would use 1 part acetone to approx. 70 parts household bleach. If this was done without an ice bath, the person performing it would now have boiling bleach on their face, and would be enveloped in a cloud of chloroform.

Essentially, that means that they'd be unconscious on the floor whilst the bleach burned their face... and then they'd die of asphyxia. :laugh:

That's why it would be done in a very small batch, and inside of a spacious ice bath.

What would occur is:

Upon adding the acetone to the hypochlorite, the solution would appear to turn cloudy. This would be the chloroform separating from the water in which the hypochlorite was dissolved. Chloroform is immiscible in water.

If this was done in a very small batch, these droplets of chloroform would remain separate due to surface tension and the presence of some impurities.  If done in a large batch, the chloroform would sink to the bottom of the vessel and accumulate into a solid blob.

Chloroform has a tendency to decompose over time, so don't attempt to keep it. It happens to decompose into Phosgene, which just so happens to be a chemical weapon... one that makes you dead. Yes, you... dead... so don't store home-made chloroform. That is unless you happen to be thoroughly educated about how to stabilize chloroform.

I honestly am not sure why I posted this, but meh... I had fun.


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Invisiblesui
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Re: Synthesizing Chloroform [Re: Konnrade]
    #5492014 - 04/08/06 05:52 AM (18 years, 1 month ago)

hahahaha


for any numbnutz reading this, DONT try it.



with that said........


....Another probobly totally useless but nonetheless cool chemistry lesson brought to you by Konnrade :grin:

i love your posts dude. :lol: Id rate you 5 right now if i didnt think ive already done it.


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InvisibleCharles
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Re: Synthesizing Chloroform [Re: Konnrade]
    #5492080 - 04/08/06 06:57 AM (18 years, 1 month ago)

Mann & Saunders, Practical Organic Chemistry, 3rd Ed

Yeah, that's Chloroform alright. It's also a really really bad idea.

Next, lets mix ammonium bisulfite with sodium hypochlorite! :tongue2:

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OfflineKonnrade
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Re: Synthesizing Chloroform [Re: Charles]
    #5492115 - 04/08/06 07:36 AM (18 years, 1 month ago)

Quote:

Charles said:
Mann & Saunders, Practical Organic Chemistry, 3rd Ed

Yeah, that's Chloroform alright. It's also a really really bad idea.

Next, lets mix ammonium bisulfite with sodium hypochlorite! :tongue2:




I don't know why, but I have an unhealthy fascination with dangerous DIY syntheses. I never perform them, but I like to talk about them... and the more likely they are to kill you, the more intrigued I get.

One of my favorites is of an unstable substance whose name I won't even mention.

My second favorite is Nitrogen Triiodide, which is even MORE unstable, but is usually made in very small quantities so as to be relatively benign. I did actually synthesize that once. I transported the wet finished product to an open area to dry... and left a cover slanted over it. I dozed off inside and when I awoke and checked on my touch powder, it had decomposed and the cover had been overturned.


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InvisibleTODAY
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Re: Synthesizing Chloroform [Re: Konnrade]
    #5492496 - 04/08/06 11:12 AM (18 years, 1 month ago)

nitrogen triodide? is that the compound that explodes when touched with a feather?


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InvisibleGratos
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Re: Synthesizing Chloroform [Re: Konnrade]
    #5494279 - 04/08/06 07:32 PM (18 years, 1 month ago)

I enjoyed hearing your DIY sunthesis and would like to hear more. How about an Ether synth or a Diethyamine extraction (if your taking requests that is). Of course a massive disclaimer shouting the dangers of these process would be in order.

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Re: Synthesizing Chloroform [Re: Gratos]
    #5495975 - 04/09/06 09:01 AM (18 years, 1 month ago)

Diethyl ether is easily produced DIY by dripping alcohol into warm concentrated sulfuric acid.

At around room temperature this happens:

2 CH3CH2-OH + H2SO4 <--> (CH3CH2O)2SO2 + H2O

Diethyl sulfate is so toxic it has been reviewed in WW I as a war gas. At elevated temperature your desired reaction takes place:

(CH3CH2O)2SO2 --decomposes--> (CH3CH2)2O + H2SO4

Here you see that your precious ether distills off and the sulfuric acid is regenerated. It acts as a catalyst. It is important to realize that you will get the diethyl sulfate impurity, so there's a trace of war gas in your ether. Overall the reaction goes like so:

2 CH3CH2-OH + H2SO4 --decomposes--> (CH3CH2)2O + H2SO4 + H2O

If you overheat the flask of sulfuric acid wherein you are dropping the alcohol an entirely different reaction takes place:

CH3CH2-OH + H2SO4 --decomposes--> CH2=CH2 + H2SO4 + H2O

In which ethylene forms. The neato thing is that your sulfuric acid is a catalyst here, between runs you just got to heat it to get rid of the water if you are making ether (not so with ethylene gas because the heat drives the water off as steam at those temperatures, making it a semi-perpetual reaction.

---

Your precious diethylamine can be made along with other ethylamines by adding some ammonia to the sulfuric acid and then adding the alcohol in the cold, so that the ethylsulfuric acid and diethyl sulfate react with the formed ammonium bisulfate like so:

2 CH3CH2-OH + 2H2SO4 + NH3 ----> (CH3CH2)2NH.H2SO4 + H2SO4.2H2O

Forming diethylamine bisulfate in diluted sulfuric acid.

The massive disclaimer is simple: DON'T DO IT!!
You are heating a highly corrosive acid, as well as causing sulfuric acid mists forming which eat away at all your tissues. On top of that the intermediate in these reactions is a nasty war gas which will end up in your end product.
So not worth it!
The chem is cool though!


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OfflineKonnrade
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Re: Synthesizing Chloroform [Re: TODAY]
    #5498360 - 04/09/06 10:58 PM (18 years, 1 month ago)

Quote:

TODAY said:
nitrogen triodide? is that the compound that explodes when touched with a feather?




Yes, yes it is.

It's a bit more stable when it's wet. Most people will make a batch of it and store it under the ammonia (or under chloroform if I remember correclty). When they want to use it they apply it to a surface and let it dry. As it dries, it becomes less stable, and kaboom!

Either something sets it off, or it just goes off on it's own after it sits for a while.

A prank I have heard of is to put a little bead of NI3 along the track of rollers in somebody's desk drawer. When they close it, it goes kaboom and the noise scares the shit out of them :evil:


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InvisibleGratos
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Re: Synthesizing Chloroform [Re: Asante]
    #5505497 - 04/11/06 08:51 PM (18 years, 1 month ago)

Quote:

The massive disclaimer is simple: DON'T DO IT!!




Yes, I completely agree. I believe if you are not skilled in synthesizing the specific molecule you shouldn't do it and if you do and are injured or killed well, you've just experienced Darwinism at it finest.

Quote:

The chem is cool though!




Yes, very cool, which is why I ask (I am not willing to risk life and limb myself and if I wanted such things, buying these [for the most part]) would be much safer and cheaper. Perhaps this is not the best place for such knowledge but is there a better place? None I have found that still exist.

Edited by Gratos (04/11/06 08:54 PM)

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InvisibleEgo Death
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Re: Synthesizing Chloroform [Re: Konnrade]
    #5511671 - 04/13/06 09:47 AM (18 years, 1 month ago)

Can u really put that stuff on a rag and knock somebody out, like in the movies?

:wink:

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OfflineKonnrade
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Re: Synthesizing Chloroform [Re: Ego Death]
    #5511911 - 04/13/06 10:57 AM (18 years, 1 month ago)

It would take a while longer than in the movies... but yeah, you could most likely do that. It's a felony, though.


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OfflineChuangTzu
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Re: Synthesizing Chloroform [Re: Ego Death]
    #5516197 - 04/14/06 02:18 PM (18 years, 1 month ago)

Your avatar makes me feel like I'm drunk. :puke:

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OfflineToboggan
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Re: Synthesizing Chloroform [Re: Konnrade]
    #5645800 - 05/18/06 10:37 AM (18 years, 5 days ago)

Very impure chloroform can be made in minutes if you skip a lot of those steps. All you have to do is add nailpolish remover(contains acetone) with Javex(dilute hpyochlorite soln) in a mason jar in an ice-bath and stir for a few minutes. The mixture will become cloudy and then blobs of chloroform will be on the bottom of the jar that you can get by decanting or pipetting. I don't remember what the proportions of acetone to bleach should be anymore unfortunately.

Its simple but its still dangerous. This should always be done in a well ventalated area with a quick escape route.

My first chloroform experiment was a disaster. A couple friends and I used bleach tablets used for swimming pools and put them in hot water to make them dissolve faster. There was a strong bleach smell for a while but then we all felt a harsh burning in our noses and throats. It was chlorine gas! We ran outside the garage coughing and gagging  until we were fit to hold our breaths and bring the jar outside. The chlorine smell eventually went away but what sucked the most was the soln didn't even work. When we added acetone there was no chloroform produced  :mad:.

So don't do it that way! I know some people are going to try to make this no matter how many people say "dont try this at home" so if you're going to then use Konnrade's method or the first one I said.

The impure chloroform can't be used for extractions but its quick to make and its fun to dissolve blocks of styrofoam with it :grin:


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OfflineManicDelirium
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Re: Synthesizing Chloroform [Re: Toboggan]
    #5652606 - 05/20/06 08:36 AM (18 years, 3 days ago)

hydrazine, check
diethylamine, check
chloroform, check
ergotamine tartrate, check



:hehehe:


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OfflineKonnrade
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Re: Synthesizing Chloroform [Re: ManicDelirium]
    #5654032 - 05/20/06 05:44 PM (18 years, 3 days ago)

Quote:

ManicDelirium said:
hydrazine, check
diethylamine, check
chloroform, check
ergotamine tartrate, check



:hehehe:




:lol:

I wouldn't trust any chloroform that was made at home to be used on something meant for ingestion. I wouldn't even trust it if I made it myself.

I've forgotten, is chloroform actually controlled at all? If not, I'd just buy the damn stuff. The hell with buying anhydrous, too... it's easy enough to make chemicals anhydrous on your own.


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Re: Synthesizing Chloroform [Re: ManicDelirium]
    #5654290 - 05/20/06 07:19 PM (18 years, 3 days ago)

Quote:

ManicDelirium said:
chloroform, check


did i miss something or did you just negate the need to synthesize?

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Invisiblecricket
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Re: Synthesizing Chloroform [Re: debianlinux]
    #5831263 - 07/07/06 11:59 AM (17 years, 10 months ago)

Well, now I know my home-built reflux tower works.
How can I find out about stabilizing and storing chloroform?


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Re: Synthesizing Chloroform [Re: cricket]
    #5831757 - 07/07/06 01:47 PM (17 years, 10 months ago)

Commercial chloroform is stabilized with pentenes (<0.01%) or ethanol (0.5-1.0%). Store it in darkness, preferably in a brown bottle.

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InvisibleDiploidM
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Re: Synthesizing Chloroform [Re: Ego Death]
    #5831890 - 07/07/06 02:12 PM (17 years, 10 months ago)

Can u really put that stuff on a rag and knock somebody out, like in the movies?

Chloroform will eventually knock someone out, but it takes many minutes, not three seconds like it does in movies. In fact, nothing you inhale will affect your brain for about 20 seconds, which is the time it takes for blood to get from your lungs to your brain.

Don't believe anything you see on TV.


--------------------
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1) You can't get married to your spouse who is the same sex as you.
2) You can't have an abortion no matter how much you don't want a child.
3) You can't have a certain plant in your possession or you'll get locked up with a rapist and a murderer.

4) We need a smaller, less-intrusive government.

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Re: Synthesizing Chloroform [Re: Diploid]
    #5834673 - 07/08/06 10:49 AM (17 years, 10 months ago)

I see how this can be dangerous.
The reaction was much more violent then I expected. A lot of heat was produced. The first time I tried it I only had cold water cooling my reflux tower. I was able to avoid the boiling bleach, but some of the chloroform vapors escaped the tower. Luck for me I was on a very well vented back porch.
I doubled the cooling coils and filled the reservoir with ice for a second run. It was interesting to watch the solution boil as the chloro condensed in the tower and poured (not dripped) back into the flask.

Don't use a syringe to collect the chloroform. It will swell the rubber and jam up. I used a chem resistant tubing to siphon it at first. That just pissed me off so I made a home-built separatory funnel out of an old fluorescent tube.


Back porch chemistry is fun. I hope I don't blow up the house.


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Invisibleblacksabbathrulz
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Re: Synthesizing Chloroform [Re: Konnrade]
    #5841293 - 07/10/06 02:18 AM (17 years, 10 months ago)

Quote:

Konnrade said:
Quote:

TODAY said:
nitrogen triodide? is that the compound that explodes when touched with a feather?




Yes, yes it is.

It's a bit more stable when it's wet. Most people will make a batch of it and store it under the ammonia (or under chloroform if I remember correclty). When they want to use it they apply it to a surface and let it dry. As it dries, it becomes less stable, and kaboom!

Either something sets it off, or it just goes off on it's own after it sits for a while.

A prank I have heard of is to put a little bead of NI3 along the track of rollers in somebody's desk drawer. When they close it, it goes kaboom and the noise scares the shit out of them :evil:




I think you are thinking of potassium tri-iodide. It forms purple crystals that are highly explosive. If you use less than pure ammonium hydroxide when you make them it is slightly safer, and takes a little more to detonate them. If you are careful you can wrap them in duct tape, and then throw them. The gas released is toxic I believe.


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InvisibleAsante
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Re: Synthesizing Chloroform [Re: blacksabbathrulz]
    #5847980 - 07/11/06 06:19 PM (17 years, 10 months ago)

Umm nope, potassium tri-iodide can be used to prepare it in quantity, but its really NI3, nitrogen tri-iodide.

You shouldn't do *anything* with NI3, other than prepare no more than 10mg on the spot where you'll explode it. It shouldnt be handled.

The NI3-in-ducttape idea is from a cookbook, and it is a BAD idea as these crystals are way too unstable to handle.

Its fun to make small projects like that but the dangers are very high. A piece of surface on which you detonate the NI3 may shoot at you several times faster than a bullet.


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InvisibleGordoTEK
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Re: Synthesizing Chloroform [Re: Asante]
    #25857888 - 03/07/19 08:29 AM (5 years, 2 months ago)

I know this is an old thread, but chloroform may actually be a useful solvent for extracting psilocybin according to things I've been researching, for example see:
http://chemistry.mdma.ch/hiveboard/rhodium/pdf/alkaloids.in.developing.shrooms2.pdf

Anyway, it is difficult to acquire chloroform, but seems relatively easy to make.  Nile Red created a video version of this here:



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Re: Synthesizing Chloroform [Re: GordoTEK]
    #25885882 - 03/20/19 02:09 PM (5 years, 1 month ago)

This thread belongs in chemistry/pharmacology.


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