Author Topic: GHB synthese  (Read 3942 times)

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icexool

  • Guest
GHB synthese
« on: October 03, 2004, 06:56:00 PM »
I've made Na-GHB today, but I can't find any clear answer to my question when searching the forums.
I did the folowing:
Dissolve 52 of NaOH in 250ml water.
And I poured 100ml y-GBL 99,7% pure into my RB flask.
And added my condenser to it to set up a reflux.
I added the hot NaOH-solution to the GBL in little portions, and a white layer formed at the bottom, I swirled it and quickly the white layer came back onto the bottom.
And I heated it to 70-80*c for 1hour, and when all the NaOH was added the white layer from the bottom got so big that there was no 2 layers anymore, and it was one layer of white suspension.
And now it has cooled all down and it pH neutral.
And there is again a white layer lying on the bottom of the flask.
Is this an oversaturated solution of Na-GHB?
In total I have 500ml solution.

http://members.home.nl/icexool/GHB1.jpg


http://members.home.nl/icexool/GHB2.jpg


http://members.home.nl/icexool/GHB3.jpg



Thanks in advance icecool.
Does anyone know what I did wrong?
I didn't even needed to add an acid to make it neutral...
I guess I added GBL in excess.

indole_amine

  • Guest
hmm
« Reply #1 on: October 03, 2004, 09:07:00 PM »
You either used too much water - or you didn't apply enough heat to your GBL before adding lye.

Also, you have to mix your GBL with a small amnt. of H2O prior to heating it (5.6ml should suffice for 100ml butyrolactone), THEN you are supposed to add the NaOH solution. And in your case, you should've used 130ml H2O to make your NaOH solution - not 250ml ...

see also

https://www.thevespiary.org/rhodium/Rhodium/chemistry/ghb-r-us.txt

...



indole_amine

icexool

  • Guest
I made GHB again today, with that method.
« Reply #2 on: October 05, 2004, 12:50:00 AM »
I made GHB again today, with that method.
And I got this, I think if I added less water yesterday and swirreled the flask hard it would have reacted...
Anyway today this:
21g NaOH+52ml water.
40ml GBL.

http://members.home.nl/icexool/GHB_good1.jpg


http://members.home.nl/icexool/GHB_good2.jpg


http://members.home.nl/icexool/GHB_good3.jpg


http://members.home.nl/icexool/GHB_good4.jpg


And a movie of how it is now, quite viscous.

http://members.home.nl/icexool/GHB_movie.mpg


indole_amine

  • Guest
90 ml?
« Reply #3 on: October 07, 2004, 01:20:00 AM »
No, the overall yield you could achieve with such amounts is ~60 grams of NaGHB, which will dissolve in little less than 120 mls of water (solubility of GHB*Na is around 0.5g/ml  ;) ). Therefore the halfway cryst. of your product...

I would advise you to make the solid NaGHB salt again, and then re-dilute it to a 0.5g/ml solution. Advantage: you know exactly about the concentration and don't have to make rather vague guesses about the strength! Further, you don't have the impurities and lactone remnants prsent, i.e. high purity product...

Try boiling off all water (and remaining butyrolactone). Heat until the temp. of the NaGHB melt reaches 150°C, then remove from heat source, and eventually place back to keep the temp between 140-150°C. Wait until nothing boils anymore - all water is evaporated now.

Then slowly pour the hot melt (use thermo gloves!) into a flat porcelain or pyrex/duran dish, trying to "pour out strips"  :)  - it will solidify almost instantly. let cool 1-2 minutes, then scrape the now solidified, very hard and shiny white NaGHB together with a metal spatula and immediately put into a sealable ziploc baggie or similar (it absorbs water from the air). You're done now!

Either weigh out the right amount each time you want to ingest some - or dilute it with water to make a "standardized stock solution" with the concentration you want: put into a clean graduated heat-resistant (duran, pyrex ot similar...) beaker let's say, 50 grams of NaGHB (of course you pulverized it with a mortar/pestle before), and add just enough hot destilled water to give a total volume of 100 ml. Add a (clean) stirbar and atir until everything has dissolved. Eventually you could again check the volume now, using a (preferably very precise) graduaded measuring cylinder, and adjust the volume to exactly 100 ml to get a solution with a concentration of incredibly precisely 0.5 grams/ml  ;)  - but this last step isn't really necessary...

(BTW the links to your pictures seem to be not working properly!?  ::) )




Does anyone know whether potassium GHB melt will form a solid upon cooling, too? Maybe higher temperatures required to dehydrate the melt properly? I assume that GHB*K is far more hygroscopic than GHB*Na, that's why I ask. If of course anyone has experienced the opposite, I would be glad to hear it, too!  :)


indole_amine

MargaretThatcher

  • Guest
KGHB
« Reply #4 on: October 07, 2004, 02:20:00 AM »
Apart from tasting better than NaGHB, KGHB is not hydroscopic. Better for your blood pressure too.

I heard that on cooling, the melt required a seed crystal, after which, crystallisation proceeded rapidly.


indole_amine

  • Guest
thanks
« Reply #5 on: October 07, 2004, 05:15:00 PM »
After waiting for 2 days, an affiliate managed to get his GHB*K to crystallize (finally, he simply cooled it and scratched - et voilà...  ;) ).

About the layers that were observed: it is normal to see layer formation during NaOH addition - it simply is the concentrated bottom water/salt/base layer, becoming immiscible with the remaining GBL top layer. As soon as most of the lye is added, it should disappear completely (nice visual indicator for when to start checking the pH, too!). But if it stays 2-layered when being cooled, you did something wong...


indole_amine

MargaretThatcher

  • Guest
K-GHB
« Reply #6 on: October 08, 2004, 03:32:00 AM »
I heard that the hot-melt crystallisation was tried once, and that it was more difficult with K-GHB than Na-GHB.

Has anyone ever tried the Mg and Ca salts? These are also non-hydroscopic and pleasant smelling according to Rhodium's page.

Maybe it would be possible to formulate an ideal Mg-Ca-K combination for the health-conscious regular user.

The recent UK classification of GHB is a travesty.


icexool

  • Guest
Well you have to go to ...
« Reply #7 on: October 08, 2004, 01:49:00 PM »
Well you have to go to

http://members.home.nl/icexool

and then click on the individual pictures.
Anyway I did it again now it boiled and everything after adding it first formed 2 layers, after shaking it started reacting heavily.
anyway it became nice clear liquid after everything was added, and I measured pH while hot (I've heard pH is different when cooled down) and so I added citric acid, and it dissolved, it became white and then the white solution disapeared and there came foam on top, and the foam went away quickly, it was only a tiny layer of foam though.
And then it still wasn't pH neutral, so added more citric acid...and then it became white again, and instantely crystals started to form...
A layer on the bottom around 1/3 of the complete volume.
It was 57ml GBL, 57ml water with 29g NaOH in the 57ml water.
Anyway I was wondering what are the crystasls?
Na-GHB or sodiumcitrate or citric acid.
My conclusion was it is Na-GHB because it dissolves well in basic enviroment, but not in neutral enviroment, so that's why it crystalized.
It will not be citric acid because it suddenly wouldn't dissolve anymore while it just a 30seconds ago did dissolve quickly and good.
You can see it on the picture this one...later on I'll upload it tonight to my ftp server.
You can now only see crappy synthese pictures of GHB because one time it is yellow the other time there was too much water.
But well I didn't make pictures of the time when the solution was completely clear.
But I do have a picture of the crystals of my GHB.
And I made a tutorial about making Na-GHB.
But I couldn't upload it but I'll try tonight again then you can exactely see what I did.
And anyway next time I'll add GBL to neutralize the excess NaOH.
Or just wait till it cooled down, a lot of people have a pH neutral GHB after it cooled down...
And no crystals. ( I wouldn't have had crystals either if I didn't add the citric acid for 90% sure) and then well maybe when it cooled down it might become milky because everyone says it is milky but my GHB was clear when warm...
But I think it would become milky when cooled down, then 2 days in refridgerator and it would become clear and ready for use (that's what I've heard)

Radiumhero

  • Guest
sounds funny....
« Reply #8 on: October 09, 2004, 07:09:00 PM »
well this Crystall Masses sound pretty funny ,When
I want to have some Ghb i just do like that:
Dissolve your NaOh / KOH in Water , get a slightly saturated solution.
when all of your KOH is added to the Water slowly start
pouring in your GBl  and get that soln neutral .
Then just evaporate most or all of the water ( use a thermometer) an cool on alufoil or something like that
in your freezer , when everything is crystalliced
just add the specific amount of water to make liquid
or put in an air tight container to store. ( Impottant when handling solid Na Ghb )
Thats it , have fun

icexool

  • Guest
Yesterday I had succes making GHB.
« Reply #9 on: October 10, 2004, 01:37:00 PM »
Yesterday I had succes making GHB.
The problems where, I did not use the stoichiometric ratio's.
And thus getting an too basic solution.
And you will need to swirl your flask very hard to get the reaction going.
Take 80% of the GBL as water and use that to dissolve the NaOH in, so if your using 50ml GBL use 40ml water and 27,86g NaOH.
With that amounts the reaction will be complete.
And do NOT add acetic acid or citric acid, there will form sodium-gamma-hydroxycitrate.
And gass will escape the butyrate as a gas.
And you will get crystals and it will just fuck up.
Only use GBL and NaOH. Measure the pH while cold not while hot the pH was 9 when it was hot and when cooled down the pH was neutral.
I got a viscous clear liquid after heavy boiling.
And I evaporated the water off and then poured it on a cold surface.
You do need to put the crystals in the oven at 110*C to get all the water out though.

indole_amine

  • Guest
layman GHB in 10 steps
« Reply #10 on: October 11, 2004, 06:13:00 AM »
Success is also guaranteed when using the following directions  ;) ...


You will need:
  • 1 thermometer capable of measuring at least 160°C
  • several pyrex/duran beakers
  • 1 measuring jug (accurate to 5 ml)
  • 1 digital scale, (accurate to at least 0.1g)
  • the notorious pyrex baking dish (or a baking plate covered with aluminum foil)
  • big-sized ziploc baggies or air-tight container

and, of course
  • gamma-butyrolactone (GBL)
  • solid NaOH (preferably ACS grade or food grade if there is any  ;) )
  • distilled H2O (no tap water please)



1. Weigh out 86.1 g GBL, put in clean beaker and add 20ml H2O to it.

2. Dissolve exactly 40.0 g NaOH in 100ml H2O.

3. Heat the GBL/H2O mixture to 105°C using a hotplate. Use the thermometer to stir it and to check the temperature. Keep at 105°C for ~10 minutes, while stirring occasionally.

5. turn off the hotplate.

4. Add the NaOH solution dropwise to the hot GBL/water mixture. Every drop will first go to the bottom and then vigorously react, producing small bubbles (boiling due to exotherm rxn).

5. After having added a certain amount of NaOH, you will see a bottom layer of NaGHB soln. and a top layer of unreacted GBL/GHB. Keep adding NaOH in little squirts, while stirring and monitoring the temp. with the thermometer.

6. When the temp. falls below 90°C, turn on the hotplate again; if it climbs to more than 110°C, remove the beaker until it is around 100°C again. Important is that the temp. is kept between 90-110°C during NaOH addition.

7. Watch the upper layer (it is somewhat cleaner than the lower salt/lye layer): you want to add NaOH solution until it has disappeared completely. So you have to slow down the addition rate as the layer gets next to nothing, and stir vigorously between the single additions. Finally, you will just see a few drops of lactone/hydroxybutyrate on top of your NaGHB solution. Drip in a few more drops of your NaOH - it shouldn't be left much of it by now.
If there is more than 10% left, your GBL wasn't pure, or you weighed incorrectly...

8. Now add 100ml H2O, and set your hotplate to maximum. Boil away the water to steam distill any unreacted lactone, remove eventual impurities derived from the GBL and to complete the reaction. No pH checking while hot/cold whatsoever...

9. The temperature will rise during steam "distillation": if it reaches the 150°C mark, you will want to keep it there; so you must remove the beaker (caution - hot!) from the hotplate and put it back on as it cools down. Continue until no bubbles evolve anymore. You now have a viscous, odorless and slightly yellowish tinted NaGHB melt. If it still smells like GBL ("sour" odor), go back to step 8.

10. Cautiously (hot!) pour the molten NaGHB into your pyrex dish or similar, trying to form strips. It will solidify almost instantly. Let cool a few minutes and scrape together the still warm NaGHB with a spatula, knife etc. If you're careful, you will be able to loosen big plates/chunks at once. Otherwise you'll have to scrape very hard, as it really sticks to the pyrex dish  :( .
Immediately place the chunks/powder into a ziploc baggie - they are very deliquescent and end up as little puddles if you wait too long...
You now have "crude" solid NaGHB.


(11. (optional))
Weigh out exactly 100 grams of NaGHB, place in beaker, and add enough H2O to give a total volume of slightly less than 200 mls. Heat under stirring until all solids have dissolved, then pour into graduaded measuring jug and adjust the volume to exactly 200ml with H2O.
(you can put a little bit food color into the water you use for volume correction, to give an appealing nice colored NaGHB solution  8) ). You now have 200mls of a nice colored 0.5g/ml NaGHB solution, ready to use, perfect for those handy-dandy 2ml PE pipettes... ;)




If it is done right, the resulting NaGHB solution is neutral (pH 7.5), with a yield of just 95%, due to small lactone losses... :)

But with this method, it is impossible to add too much NaOH, and impossible to have remaining lactone contaminations as well. The product in solution will in fact be odor- and tasteless! (Promised!)  8)



indole_amine

indole_amine

  • Guest
almost perfect
« Reply #11 on: October 11, 2004, 02:00:00 PM »
The purpose of adding water to the GBL (and heating it) is to hydrolyze it to GHB.

When you add your NaOH solution dropwise, the reaction doesn't become too exothermic, and you have a good visual control about what's going on. But if all is added at once, the temperature will rise too high, and some GHB/GBL will evaporate. Result is a too basic solution then, therefore you then have to add more GBL...

Try heating the GBL with some water first, and then add the NaOH solution dropwise. Everything else in your writeup seems absolutely correct.  ;)


indole_amine

hypo

  • Guest
Ghetto-GHB
« Reply #12 on: October 11, 2004, 02:17:00 PM »
of course (sorry, for i'm repeating myself) in a ghetto situation, and i have
a feeling that's what we're talking about here, usage of sodium bicarbonate
(baking soda) or sodium carbonate (washing soda) is preferable over hardware
store NaOH.

this eliminates the risk of alkali burn or poisoning.

matter of fact: i taught how to perform this reaction to an opiate addict (in a
pot and with a wooden spoon!) and it works pretty well.


indole_amine

  • Guest
ain't no ghetto GHB...
« Reply #13 on: October 11, 2004, 03:36:00 PM »
Well if you'd clicked on the link to the tutorial Icexool made, you would know that there was no "ghetto situation" - he used analytical grade NaOH and GBL, further he has all necessary equipment to properly perform htis reaction (which ain't much  ;) ).

Of course, food grade sodium bicarb is the better choice than tech grade NaOH; but washing soda?? Doesn't sound like it would be healthier than drain cleaner, if you ask me...

Alkali burn or poisoning can't happen if you follow my instructions: as there is a slight excess GBL present even after having added the last lye (excess GBL is then removed by steam distillation).


indole_amine

hypo

  • Guest
sorry...
« Reply #14 on: October 11, 2004, 03:41:00 PM »
...i refuse to click on external links. maybe if he uploads it here...

anyway, maybe icexool has analytical grade NaOH, most bees don't so i
let my post stand as it is. better one heads up too much.

> but washing soda?? Doesn't sound like it would be healthier than drain cleaner,
> if you ask me...

sounds evil, but it's pure sodium carbonate.

> Alkali burn or poisoning can't happen if you follow my instructions

you're in the newbee forum. why risk anything!?


indole_amine

  • Guest
paranoid? ;^)
« Reply #15 on: October 11, 2004, 04:23:00 PM »
i refuse to click on external links. maybe if he uploads it here...

Why - paranoid?  ;)  But I just mailed Icexool instructions on how to upload files to the Hive, hopefully he makes use of them!  :)

you're in the newbee forum. why risk anything!?

You're right - noone knows how much people can fuck up with simple rxns (re: RP/I)  ;) ...

BTW would you recommend to use bakin/washing soda in solution, too - or might it bee wise to add it in solid form (as it reacts not as readily as NaOH)?


indole_amine

hypo

  • Guest
yep...
« Reply #16 on: October 12, 2004, 12:39:00 AM »
> Why - paranoid?

yes.  :P

> But I just mailed Icexool instructions on how to upload files to the Hive,
> hopefully he makes use of them!

thank you.

> You're right - noone knows how much people can fuck up with simple rxns (re: RP/I)

indeed. i've been reading the newbee forum practically daily for years now and what
i've seen people eat is amazing: brown stuff, stinking stuff, wet stuff, corrosive
stuff (yes, burnt tongues, more than once!), stuff that tastes like table salt (a classic!),
poppy seed extract, and that's only what i remember... in their desparation to get high,
people will do anything.

> would you recommend to use bakin/washing soda in solution, too - or might it bee wise to
> add it in solid form (as it reacts not as readily as NaOH)?

i've done this reaction only once in controlled setting (with flask and condensor), what i
did was add the carbonate, water (search chromic's posts for the right amount) and GBL,
then turn on heat and stirring (stirring didn't work at first, since i was using 500g of
bicarbonate). the carbonate goes slowly into solution and the reaction took about 24h to
complete.

in ghetto setting, it's the same, but pot instead of flask, spoon instead of stirrer and
about 3h on a stove. in the end the solution is heated until it reaches 150C. of course this
way there are losses, but no hurt GHB-user.


indole_amine

  • Guest
CO2?
« Reply #17 on: October 12, 2004, 01:41:00 AM »
Did you have any problems with foaming (especially your ghetto friend  :) )? If 500g bicarb release their carbonate moiety in only 3h under heating, there should be a *lot* of CO2 formed(?)

(attention newbees - watch out for boilovers here!  ;) )


indole_amine

hypo

  • Guest
actually there was no problem
« Reply #18 on: October 12, 2004, 01:59:00 AM »
the pot was only half filled and that was smaller reactions.
i don't know the exact number anymore, but they were in the 100-200g
(GBL or carbonate) range. there's a steady evolution of CO2, which is
very easily controlled by adding / removing heat.


icexool

  • Guest
upload
« Reply #19 on: October 12, 2004, 06:06:00 AM »
As asked before I'll upload the GHB synthese on the hive server.
Here it is,


Hope you like it and please comment.