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Chemrock
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Distillation Setup for 1,4-Butanediol to gamma-Butyrolactone
Any recommendations on the easiest distillation apparatus setup for distilling GBL from a filtered BDO+CuCrO4 slurry ?
I have cooked the BDO and the CuCrO4 for 3 hours at 200 deg C, and have filtered the majority of the CuCrO4 out via a coffee filter. Now I need to
distill to obtain the GBL.
[Edited on 3-1-2010 by Chemrock]
[Edited on 3-1-2010 by Chemrock]
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User
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Cooking.......................?
Forget it man.
Cooks are like rats , they dont die easily.
[Edited on 3-1-2010 by User]
What a fine day for chemistry this is.
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Chemrock
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Sorry I should have said refluxed instead of cook, my bad
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DJF90
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Take your pots and pans elsewhere; we aren't interested in helping your kind!
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entropy51
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If you don't how to set up a distillation setup
and you're trying to make GBL, you're probably a cook no matter how you say it.
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Chemrock
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There are a lot of ways to set up a distillation. My question was as to the simplest for the process I described based on anyones experience. For
example is it necessary to perform fractional distillation in the process. What type of condenser would be sufficient, ie West, Graham,Liebig etc. Is
it necessary to water cool or can air cool suffice.
For example would the setup shown on this link be sufficient:
http://www.unitedglasstech.com/Monthly_Specials.htm
Thanks for any advice
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turd
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I don't know that particular synthesis, but I guess ideally you would use a small column (10-20 cm). A glass blower will make you a Hempel column for
~$20. Apart from that the apparatus you posted looks nice. Also I'm not sure how stable gamma-hydroxybutyrolactone (GBL) is. In case it is unstable at
higher temperatures you might want to use a vacuum source, an aspirator should do. Of course you need a good heat source and preferably a magnetic
stirrer.
Edit: An important aspect is the scale you're operating on. If you're working on the 10g scale, you need special "micro" distillation apparatuses. For
100g batches the posted apparatus should be fine, but additional 100ml and 250ml round bottom flask would be a nice thing to have.
PS: I wonder if an industrial solvent like GBL is worth the trouble - but it sounds like a nice first chemistry project. 
PPS: The witch-hunt here is getting to ridiculous levels. From the FAQ:
| Quote: | Mad Science is about [...] Things Man was Not Meant to Know. More prosaically, Mad Science is about exploring and manipulating aspects of the natural
world without the facilities or resources of "sane science" as practiced in academic, industrial, and governmental research settings.
[...]
Mad Scientists are drawn like moths before a candle to the most dangerous areas of exploration: energetic, corrosive, and bioactive
materials. |
Sounds like Chemrock is more in the spirit of the site than the academic wanks... 
[Edited on 3-1-2010 by turd]
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User
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Also to help someone clueless that just after a direct precursor to GHB...
Right..
What a fine day for chemistry this is.
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entropy51
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From the FAQ: | Quote: | | It is okay to be ignorant when first arriving and posting. However, you must be willing to make an effort to learn. Additionally, certain topics are
unwelcome no matter what section they are posted in. The discussion of criminal activities or weapons production is inappropriate. Heed this
warning or face merciless taunting. |
GBL is a List 1 Chemical.
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Chemrock
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I've noticed
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turd
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*shrug*
Where I live its legal to possess (and make) unlimited amounts of GBL as long as it's stored correctly. So your "List 1" might not be as important as
you think.
Back on topic: The plastic clamps suck, I've managed to melt those during distillation. Get ones made from metal.
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entropy51
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Quote: Originally posted by turd  |
Where I live its legal to possess (and make) unlimited amounts of GBL as long as it's stored correctly. So your "List 1" might not be as important as
you think. |
Sez you. Chemrock says he's in San Francisco, and it's not legal there. The taunting will continue.
Polverone, could we get a better class of cooks around there? GHB is such crap.
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Chemrock
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Based on the number of views this topic has generated I would say that my interest is shared by many. After all it is a "discussion board" not an
interview forum for the next Pope
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entropy51
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| Quote: Originally posted by Chemrock | | Based on the number of views this topic has generated I would say that my interest is shared by many. After all it is a "discussion board" not an
interview forum for the next Pope |
WTF, you're not just a newbie, you're dense too. Views? Try looking at
the posts. Not exactly a heartwarming response, huh?
Views? Most drivers slow down to gawk at auto accidents. I suppose you believe all of them think highway fatalities are a good thing and aspire to
become one.
[Edited on 3-1-2010 by entropy51]
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Chemrock
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The world is full of pleasant people unfortunately you're not one of them.
"Better living through chemistry"
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entropy51
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Good grief! If you think me not pleasant, you wouldn't enjoy the comaraderie of a prison at all, so maybe you should refrain from naughty chemistry,
lest you get yourself locked up in a very unpleasant place.
[Edited on 4-1-2010 by entropy51]
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Sedit
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LOL sorry buddy but I must laugh.... He really said "Cooked the BDO" LMAO, sorry but that is to funny.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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DJF90
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Hahahaha good one entropy... I actually had a U2U exchange with this guy after he was complaining about my post to him... well it looks like he took
some notice of what I said and has cleaned up a little... but seriously... GBL? I can think of nicer, and more legitimate ways of getting into amateur
chemistry.
Chemrock: If you're serious about getting into chemistry as an amateur hobby, then stick around. Just chose some more sane projects and you'll be a
lot better off, people will be more interested in your work and you'll get alot from it. A good set of glass with ground joints is pretty essential if
you're into serious organic synthesis, and will prove valueable over time if not instantly.
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JohnWW
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I suppose Chemrock's philosophy is: "If something is illegal, it must be good for you". There is some truth in this, however, because in many places
drugs, including ones with analgesic or naturopathic or other pharmacological value, including non-alkaloidal ones like 1,4-butanediol and GBL and GBH
and pot, have been made illegal by an abuse of legi$lative process, in the form of massive lobbying and bribery (often disguised as "election campaign
contributions") of Congre$$people (particularly in the U$A) and Parliamentarians by the big alcohol and tobacco and pharmaceutical companies, who see
such rival drugs as threats to their "patches", i.e. to their own grossly-overpriced wares.
BTW, there is not really much point in converting 1,4-butanediol to GBL, to use as a recreational drug, because 1,4-butanediol (which is made
industrially in large quantities for use as an industrial solvent, which should be in Ullmann) itself can be drunk for the same drug effect,
comparable to ethanol.
[Edited on 5-1-10 by JohnWW]
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psychokinetic
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I could really go a good, relaxing, refreshing murderous spree right now.
“If Edison had a needle to find in a haystack, he would proceed at once with the diligence of the bee to examine straw after straw until he found
the object of his search.
I was a sorry witness of such doings, knowing that a little theory and calculation would have saved him ninety per cent of his labor.”
-Tesla
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turd
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Actually that's close to the perfect project for an absolute beginner in organic chemistry:
* Harmless reagents
* Cheap reagents
* Refluxing
* Catalysis
* Distillation
* Not too small of a scale
In any case, definitely better than my career starter: chloroform and chloral-hydrate.
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Sedit
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[rquote=168880&tid=13208&author=turd
Actually that's close to the perfect project for an absolute beginner in organic chemistry:
* Harmless reagents
* Cheap reagents
* Refluxing
* Catalysis
* Distillation
* Not too small of a scale
In any case, definitely better than my career starter: chloroform and chloral-hydrate.[/rquote]
See turd the issue is people inhearited belief in what harmless means. There is also the issue of someones ability to make a consumable product
without proper understanding and facilitys. But hey who the hell am I to judge im just putting the facts of the matter out there.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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len1
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The sad truth is, if you made anything, be it drug related, be it bomb related, just anything, having it reality related would already make it above
par on this forum
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Sedit
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Put that way len it sort of depresses me. I like to feel this is a forum of people who may have had experiance with the sometimes dangerous stuff I
play with. If something goes wrong I would like to have somewhere to turn other then what I can look up on google myself.
If people are reading and not practicing there is no excuss IMO because money is no huge factor and with a little ingenuity alot of equipment can be
made from things in the shed. Small projects can be performed and down the line these can be combined into bigger projects given puritys and abilitys.
:Sigh: stop depressing people Len
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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len1
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| Quote: |
If people are reading and not practicing there is no excuss IMO because money is no huge factor and with a little ingenuity alot of equipment can be
made from things in the shed. Small projects can be performed and down the line these can be combined into bigger projects given puritys and abilitys.
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I agree with you entirely. Unfortunately the only people who want to get off their butt and do the unglamorous work are those with a vested interest.
i.e. drug cooks and bomb makers. This is the reason for an observation of Polverone's earlier that SM can never reach the level of the Hive. What
united them there is a common purpose.
Depressing - yes, I find it depressing. But I cant find solace in an imaginary reality. Maybe others can, maybe its to their benefit, maybe its not
so bad, so I will stop intruding.
[Edited on 5-1-2010 by len1]
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