Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1  
Author: Subject: Distillation Setup for 1,4-Butanediol to gamma-Butyrolactone
Chemrock
Harmless
*




Posts: 8
Registered: 18-10-2009
Location: San Francisco, CA USA
Member Is Offline

Mood: Mellow

[*] posted on 3-1-2010 at 09:52
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]
View user's profile View All Posts By User
User
Hazard to Others
***




Posts: 339
Registered: 7-11-2008
Location: Earth
Member Is Offline

Mood: Passionate

[*] posted on 3-1-2010 at 10:02


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.
View user's profile View All Posts By User
Chemrock
Harmless
*




Posts: 8
Registered: 18-10-2009
Location: San Francisco, CA USA
Member Is Offline

Mood: Mellow

[*] posted on 3-1-2010 at 10:20


Sorry I should have said refluxed instead of cook, my bad
View user's profile View All Posts By User
DJF90
International Hazard
*****




Posts: 2266
Registered: 15-12-2007
Location: At the bench
Member Is Offline

Mood: No Mood

[*] posted on 3-1-2010 at 10:30


Take your pots and pans elsewhere; we aren't interested in helping your kind!
View user's profile View All Posts By User
entropy51
Gone, but not forgotten
*****




Posts: 1612
Registered: 30-5-2009
Member Is Offline

Mood: Fissile

[*] posted on 3-1-2010 at 10:59


Quote: Originally posted by Chemrock  
Sorry I should have said refluxed instead of cook, my bad
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.
View user's profile View All Posts By User
Chemrock
Harmless
*




Posts: 8
Registered: 18-10-2009
Location: San Francisco, CA USA
Member Is Offline

Mood: Mellow

[*] posted on 3-1-2010 at 11:15


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

View user's profile View All Posts By User
turd
National Hazard
****




Posts: 800
Registered: 5-3-2006
Member Is Offline

Mood: No Mood

[*] posted on 3-1-2010 at 11:36


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]
View user's profile View All Posts By User
User
Hazard to Others
***




Posts: 339
Registered: 7-11-2008
Location: Earth
Member Is Offline

Mood: Passionate

[*] posted on 3-1-2010 at 11:58


Also to help someone clueless that just after a direct precursor to GHB...
Right..




What a fine day for chemistry this is.
View user's profile View All Posts By User
entropy51
Gone, but not forgotten
*****




Posts: 1612
Registered: 30-5-2009
Member Is Offline

Mood: Fissile

[*] posted on 3-1-2010 at 12:26


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.:P

View user's profile View All Posts By User
Chemrock
Harmless
*




Posts: 8
Registered: 18-10-2009
Location: San Francisco, CA USA
Member Is Offline

Mood: Mellow

[*] posted on 3-1-2010 at 12:44


I've noticed
View user's profile View All Posts By User
turd
National Hazard
****




Posts: 800
Registered: 5-3-2006
Member Is Offline

Mood: No Mood

[*] posted on 3-1-2010 at 13:00


*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. :P Get ones made from metal.
View user's profile View All Posts By User
entropy51
Gone, but not forgotten
*****




Posts: 1612
Registered: 30-5-2009
Member Is Offline

Mood: Fissile

[*] posted on 3-1-2010 at 14:40


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.
View user's profile View All Posts By User
Chemrock
Harmless
*




Posts: 8
Registered: 18-10-2009
Location: San Francisco, CA USA
Member Is Offline

Mood: Mellow

[*] posted on 3-1-2010 at 14:45


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
View user's profile View All Posts By User
entropy51
Gone, but not forgotten
*****




Posts: 1612
Registered: 30-5-2009
Member Is Offline

Mood: Fissile

[*] posted on 3-1-2010 at 14:51


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]
View user's profile View All Posts By User
Chemrock
Harmless
*




Posts: 8
Registered: 18-10-2009
Location: San Francisco, CA USA
Member Is Offline

Mood: Mellow

[*] posted on 3-1-2010 at 14:56


The world is full of pleasant people unfortunately you're not one of them.



"Better living through chemistry"
View user's profile View All Posts By User
entropy51
Gone, but not forgotten
*****




Posts: 1612
Registered: 30-5-2009
Member Is Offline

Mood: Fissile

[*] posted on 3-1-2010 at 15:17


Quote: Originally posted by Chemrock  
The world is full of pleasant people unfortunately you're not one of them.


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.:o

[Edited on 4-1-2010 by entropy51]
View user's profile View All Posts By User
Sedit
International Hazard
*****




Posts: 1939
Registered: 23-11-2008
Member Is Offline

Mood: Manic Expressive

[*] posted on 3-1-2010 at 15:52


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
View user's profile View All Posts By User
DJF90
International Hazard
*****




Posts: 2266
Registered: 15-12-2007
Location: At the bench
Member Is Offline

Mood: No Mood

[*] posted on 4-1-2010 at 13:37


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.
View user's profile View All Posts By User
JohnWW
International Hazard
*****




Posts: 2849
Registered: 27-7-2004
Location: New Zealand
Member Is Offline

Mood: No Mood

[*] posted on 4-1-2010 at 13:56


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]
View user's profile View All Posts By User
psychokinetic
National Hazard
****




Posts: 558
Registered: 30-8-2009
Location: Nouveau Sheepelande.
Member Is Offline

Mood: Constantly missing equilibrium

[*] posted on 4-1-2010 at 14:03


Quote: Originally posted by JohnWW  
"If something is illegal, it must be good for you".


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
View user's profile View All Posts By User
turd
National Hazard
****




Posts: 800
Registered: 5-3-2006
Member Is Offline

Mood: No Mood

[*] posted on 4-1-2010 at 15:04


Quote: Originally posted by DJF90  
GBL? I can think of nicer, and more legitimate ways of getting into amateur chemistry.

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.
View user's profile View All Posts By User
Sedit
International Hazard
*****




Posts: 1939
Registered: 23-11-2008
Member Is Offline

Mood: Manic Expressive

[*] posted on 4-1-2010 at 17:40


[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
View user's profile View All Posts By User
len1
National Hazard
****




Posts: 595
Registered: 1-3-2007
Member Is Offline

Mood: NZ 1 (goal) - Italy 1 (dive)

[*] posted on 4-1-2010 at 18:43


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
View user's profile View All Posts By User
Sedit
International Hazard
*****




Posts: 1939
Registered: 23-11-2008
Member Is Offline

Mood: Manic Expressive

[*] posted on 4-1-2010 at 21:41


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
View user's profile View All Posts By User
len1
National Hazard
****




Posts: 595
Registered: 1-3-2007
Member Is Offline

Mood: NZ 1 (goal) - Italy 1 (dive)

[*] posted on 4-1-2010 at 22:20


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.


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]
View user's profile View All Posts By User
 Pages:  1  

  Go To Top