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/GHB1.jpg)
http://members.home.nl/icexool/GHB2.jpg (http://members.home.nl/icexool/GHB2.jpg)
http://members.home.nl/icexool/GHB3.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.
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 (https://www.thevespiary.org/rhodium/Rhodium/chemistry/ghb-r-us.txt)
...
indole_amine
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_good1.jpg)
http://members.home.nl/icexool/GHB_good2.jpg (http://members.home.nl/icexool/GHB_good2.jpg)
http://members.home.nl/icexool/GHB_good3.jpg (http://members.home.nl/icexool/GHB_good3.jpg)
http://members.home.nl/icexool/GHB_good4.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 (http://members.home.nl/icexool/GHB_movie.mpg)
Well you have to go to http://members.home.nl/icexool (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)
As asked before I'll upload the GHB synthese on the hive server.
Here it is, (https://www.thevespiary.org/rhodium/Rhodium/hive/hiveboard/picproxie_imgs/pdf.gif)
Hope you like it and please comment.