Author Topic: GBL -> GHB yield question  (Read 2403 times)

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noj

  • Guest
GBL -> GHB yield question
« on: April 03, 2002, 06:18:00 PM »
I've seen statements saying that conversion is in the 60-70% range (Erowid, Rhodium's), leaving some unreacted GBL. If the pH is neutral after the reaction, and molar ratios were used, what happens to the unreacted NaOH or KOH? How does it become pH neutral if all of the GBL doesn't react?

Everyone falls down. It's how fast you get back up that is important.

Rhodium

  • Guest
GHB Yield
« Reply #1 on: April 03, 2002, 07:44:00 PM »
The yield is quantitative if you mix the reactants and keep them in the original solution, but if you are attemting to isolate the dry, purified Na-GHB solid as a salt, then your yield might be 60-70% because it is so water-soluble.

noj

  • Guest
GBL to GHB questions
« Reply #2 on: April 03, 2002, 08:33:00 PM »
This goes against everything I've read so far, but makes sense. I wonder why there are so many statements regarding the unreacted lactone, in taste or smell.  Even the write-up's mention it will be left there, in some amount. Does the GHB revert back to GBL or something?

Is heating to 150°C until half the reaction contents remain needed? This is then diluted again to the desired percentage.

Everyone falls down. It's how fast you get back up that is important.

Chromic

  • Guest
quantitative yield
« Reply #3 on: April 04, 2002, 01:55:00 AM »
The yield is quantitative if you use the following synthesis: add 1 mol of NaHCO3, NaOH or KOH and 1 mol of GBL... add a fair amount of distilled water. Reflux it until the pH is neutral, then boil it until the liquid reaches 150C. Then pour it in strips onto a cold metal surface (eg teflon-coated cookie tin), it will crystallize, and break it off. Store it in an air tight container. This procedure works wonderfully for making solid NaGHB.

spectralmagic

  • Guest
MeOH instead of H2O
« Reply #4 on: April 04, 2002, 10:14:00 AM »
SWISM uses a similar method, but in MeOH instead of H2O.  Reflux, adjust pH (it's almost always a little on the basic side, even with careful measuring before mixing), you will get a flurry of teeny tiny white specs as the pH approaches neutral (is GHB-salt more soluble in basic solutions, and precipitates out when made neutral?), boil off MeOH (until no more bubbles), let solidify.  You get white waxy chunks of solid GHB-salt with practically no salty taste when dissolved in water... there is some taste, hard to describe, but not a lactone taste, and not the intense salty taste you get if you heavily adjust pH and keep it all in an aqueous solution.

It works every time... but bee careful if you're evaporating the MeOH in your oven... even an electric one.  SWISM had a memorable event a while back where he almost lost the oven door, the electric heating element was hot enough to ignite the "fuel-air bomb" that had formed.  :o   Boiling away from ignition sources seems to be the way to go (beware of electric fans with sparking contacts in their motors!), don't let the vapours build up!

Edit: SWISM's yields have always been 99%+...  some mechanical losses are inevitable.  Except for that one time with the fire... product was discoloured, SWISM washed with acetone & recrystalised, yielded about 90%, but he was happy to be alive, yet alone still get product!

To Bee, or not to Bee...  ;-)

slothrop

  • Guest
Re: you will get a flurry of teeny tiny white ...
« Reply #5 on: April 04, 2002, 10:28:00 AM »

you will get a flurry of teeny tiny white specs as the pH approaches neutral (is GHB-salt more soluble in basic solutions, and precipitates out when made neutral?)




As the pH approaches neutral more Na-GHB have been formed and it crashes out since the refluxing MeOH can't hold it.

//Tyrone Slothrop



Chromic

  • Guest
H2O over MeOH
« Reply #6 on: April 04, 2002, 06:08:00 PM »
Given the choice of evaporating water or methanol, I'll let the readers decide which they'd prefer to use... especially after your story of a fire...

foxy2

  • Guest
LOL
« Reply #7 on: April 04, 2002, 07:18:00 PM »
"but bee careful if you're evaporating the MeOH in your oven"

Is that not an oxymoron?
;D


But I would still rather evap methanol, than evap H2O.
With proper precautions its no big deal, and way faster.

Those who give up essential liberties for temporary safety deserve neither liberty nor safety

Chromic

  • Guest
Huh? No way!
« Reply #8 on: April 04, 2002, 11:24:00 PM »
Foxy, how do you safely and easily evaporate to dryness a large quantity of MeOH (say ~5-10L) to recover solid GHB? (don't say rotovap or fumehood because you're aware neither of those approaches are satisifactory answers)

With water, one just puts it into a sauce pan on the stove, cranks the heat, turns on the exhaust fan...

foxy2

  • Guest
here is how
« Reply #9 on: April 05, 2002, 12:06:00 AM »
big flask/pot and an aspirator hooked up to a funnel sitting on top.  Funnel is quasi fumehood, semi-sealed but not tight enough to draw a vacuume just enough to get all the vapor.

How THAT???
:P  :P  :P  ;D



Those who give up essential liberties for temporary safety deserve neither liberty nor safety

foxy2

  • Guest
Or this
« Reply #10 on: April 05, 2002, 12:11:00 AM »
Do it outside on low heat while forceing air into the solution or blowing air over it(to speed evap)

I am unsure of the heat liability of the GHB, but that shouldn't be an isssue while evaping the first 95+% of the methanol.

Those who give up essential liberties for temporary safety deserve neither liberty nor safety

noj

  • Guest
GHB first time
« Reply #11 on: April 05, 2002, 06:04:00 AM »
Well, after getting confirmation, I tried this juice for the first time. It tasted slightly salty, but not like I was thinking it would. Made using KOH, it had a slight salt aftertaste, followed by a numbing and slight sting. The numbing persisted, similar to burning your tongue with coffee. This led me to think maybe it was still caustic, so a pH test was done. It read 6.8. Odd, so I tested some distilled water and it was 6.8, so my meter was wrong. Read the responses here and then decided to consume 15mL, equiv to 3g of salt. After 15 minutes, I felt a little spacey. After 30 minutes, I felt pretty good, and then a short while after I felt pretty drunk, but without the alcohol side effects. The state lasted about an hour and a half, then retired to the bedroom for some carnal knowledge, which was fast and furious  :-[ . After reaching a somewhat normal state, I felt relaxed and content. The next day was chipper, with no hang over or anything.

Is this a typical experience or can more be tolerated safely? I know the Potassium salt is less active by weight. I have heard the typical experience is nodding out briefly, then being high and horny. All I felt was lack of visual focus, slightly drowsey, but not sleepy.

Mastery is based on the understanding and practice of technique.

spectralmagic

  • Guest
Good on ya!
« Reply #12 on: April 05, 2002, 08:36:00 AM »
noj,

Work it up 250mg at a time (no, not on the same day!).  SWISM eventually arrived at a rather pleasant not-quite-passing-out dose of 42.3mg/kg (in his case that's about 5g of NaGHB)...  that works out to 47.1mg/kg if using KGHB.

SWISM would be very interested to hear your comparison of NaGHB to KGHB, if you ever get the chance to try both.  He harbours a suspicion that the potassium inhibits the euphoria somehow...  his first time was with NaGHB, 4g and then another 4g 60 minutes later (do NOT do this!), absolutely fantastic, until he passed out...

Post 286281 (missing)

(newguyhere: "is this what MDMA "loss of magic" feels like?help!", General Discourse)
, scroll about half-way down, some discussion of KGHB there.
Post 280942 (not existing), another "informative" thread  ;D

And regarding SWISM's little explosion and consequent little fire...  he now boils down on a hotplate with a fan blowing towards the mix, so the fumes blow away without encountering the sparking motor.  This doesn't occur outside (too many prying eyes), but it is a very well ventilated room.  No more surprises since.

Edit: Just noticed the "Hive Addict" title, you've probably already read those threads.  ;)   And for fear that this post has drifted into the dreaded sea of off-topica, I'll shut up now.

To Bee, or not to Bee...  ;-)

noj

  • Guest
MeOH as solvent
« Reply #13 on: April 05, 2002, 03:46:00 PM »
Isn't there a fear of contamination using this? Or are we talking about lab grade MeOH?

Mastery is based on the understanding and practice of technique.

Sunlight

  • Guest
Easier
« Reply #14 on: April 05, 2002, 06:32:00 PM »
I don't know why you wnat to complicate the things. First time I made GHB I used methanol and recovered solid product, and it was interesting, but it's much more practicla to do it in water and make a soltion with the adequate concenjtration, it's easier and it's the same. Furthermore solid GHB is so hygroscopic that if you don't care it a lot it will be a syrupe in minutes. My oppinion is that for getting the same, easier ways are better ways.

StraightEdge

  • Guest
It's not THAT hygroscopic
« Reply #15 on: April 07, 2002, 04:01:00 AM »
My friend has had solid GHB stored in a platic bag for almost a year now. Curiously, it has retained its solid form.