The Vespiary

The Hive => Newbee Forum => Topic started by: killerbeezzz on October 18, 2004, 04:03:00 PM

Title: Freebase Stablity
Post by: killerbeezzz on October 18, 2004, 04:03:00 PM
Swim has 30ml of raw MDMA freebase that is diluted with 150ml of DCM.  The problem is that swim can not distill it for a week.  He is wondering if putting it in the freezer is the way to maintain the stability of his freebase?  Also Swim if planning on using the Brightstar crystallization method.  The issue that Swim has there is that is is supposed to be anhydrous but the directions say to add Muric acid and that contains water.  Does Swim need to find a different source of HCL?
Title: should not be a problem
Post by: DoctorFeelgood on October 18, 2004, 04:11:00 PM
freezing for a week should not be a problem. i would recommend to dissolve the distilled freebase in xylene or toluene, then gas with HCl (e.g. NaCL + HCL + H2SO4).
Title: Gassing advantages?
Post by: killerbeezzz on October 18, 2004, 05:51:00 PM
What are the advantages of gassing verses the BS meathod?  Will I get a better yeild?
Title: as long as it is stored in NP and placed in...
Post by: ApprenticeCook on October 18, 2004, 10:54:00 PM
as long as it is stored in NP and placed in freezer your fb will be fine for a week....

as for gassing methods UTFSE as the options have been done to death and it has been shown everyone has their own opinion on the issue....

How did you get this far without knowing your gassing method? thats the easiest part!


Title: Getting Places
Post by: killerbeezzz on October 18, 2004, 11:52:00 PM
This attempt is SwiK's second attempt at the Al/Hg via the MM method.  He followed the directions in the MM method writeup to the T the first try. When it came time to gas he had not done an A/B extraction.  Nor had he distilled the freebase.  When he gassed the toluene all that happened was it got cloudy for a minute.  Then it went clear again after a few hours of sitting in the freezer there was brownish oil at the bottom with crystals growing out of it.  After 2 days he harvested the crystals and tasted them.  It ended up being about 5g of MDMA.  This time he did a few recommended changes to the MM method.  That included letting the Al amalgamate longer before starting the nitro/ketone dripping, pre charging the amalgamation with 3ml of nitro, and refluxing for 2 hours after the nitro/ketone addition was finished.  Then he did the work up on the toluene with four 500ml dH2O washes and one 500ml saturated NaCl wash.  Then he did a A/B extraction with 200ml of 10% hcl and then basified that with 150ml of 20% NaOh solution.  Once the PH was at 12 he stopped basifying the aqueous layer was a milky white with very light brown oil at the bottom of the sep funnel.  He added 50ml of DCM and shook for 2 min and dropped the DCM and oil layer out of the funnel.  He then did five more 50ml DCM washes.  He is wondering if there might be more freebase in the toluene because it still smells like ketone and is a little cloudy.  Should he try a second A/B on the existing toluene?
Title: one word.... PARAGRAPHS Ok, so you extracted...
Post by: ApprenticeCook on October 19, 2004, 05:25:00 PM
one word.... PARAGRAPHS

Ok, so you extracted the post amalgum mix (disgusting shit) with toly... then you did a brine wash and water wash, good.

Did you sep off the aqueous layer?

You A/B the toly, and...
Once the PH was at 12 he stopped basifying the aqueous layer was a milky white with very light brown oil at the bottom of the sep funnel
the toly would sit at the top of the water.... you had three layers? this has gotten me confused.... or am i reading it wrong?
Your A/B'd toly should be on the top of the aqueous layer, then the milky aqueous layer, THEN you had a light brown oil at the bottom of the aqueous layer???

So you DCM extracted the light brown oil.... do a few more and pool the extracts, make sure you agitate the mix and then leave for a few mins for the layers to adequatly seperate before you sep off....

I wouldnt do another A/B you seem to have done enough, and yes there may be more ketone left unreacted in the toly post amalgum so distill it and find out, more than likely its only a tiny amount (trace) thats giving the smell....

There may well be fb in toly still, but the FB is more soluble in DCM than toly (right??) so if there is it will only be a small amount, sep off the aqueous layer and DCM extract the toly a few times, pool the extracts with your others and distill off the DCM, then setup for vacuum distill and distill the freebase... then gas.

Should be right after that....


Title: One last thing
Post by: killerbeezzz on October 19, 2004, 05:58:00 PM
I am sorry I didn't explain his procedure well.  He A/Bed the toly with 200ml of 10% Hcl.  Then in the sep funnel seperated the aqueous layer from the toly.  He then basified the aqueous layer with a 20% NaOh soulution till the target PH of 12 was reached.  At that time about 30ml of very light brown oil fell out of soulution. and the aqueous layer was a milky white. 

Using three washes of 50ml each he washed the basic aqueous soulution.  After each wash he allowed the layers to resolve for 5 minutes or untill a clean line was between the layers.  Then he tapped off the DCM and pooled it with the other DCM washes and the oil.  That is were he is at right now. 

What he is trying to figure out is either to gas or use the IPA/Xylene Meathod of Crystalization.  He has trie the gassing with no luck on a previous run but at the same time he didn't A/B or distill the freebase.  After the DCM is distilled off and the freebase is distilled how much Xylene should he use when gassing?  He has UTFSE and most ppl are saying from 1 part FB to 4 parts NP or a 1 to 8 ratio.  So he is abit confused.  Also how quickly should he gass the soulution should it just be a slow bubble or a stream of bubbles?
Title: sounds ok from what im reading....
Post by: ApprenticeCook on October 22, 2004, 08:38:00 AM
sounds ok from what im reading....

a very common source of error in gassing is not having it dry... you need to be paranoid about moisture in the gas and in the fb/np mix....
You can try the IPA/Xylene titration if you want, either works fine but i find gassing easier....

For solvent, i use 1 part fb to 4 parts np, but you may need to adjust it slightly. You need enough so your crystals can form nicely without being crowded.

Gas rate, well about ~3 bubbles / sec is good, adjust rate by increasing or decreasing gas generator drip speed.

See how you go. If you gas make sure everything is dry!