Author Topic: Bromosafrole success with PTC - Jon's method does NOT work ! (Read 1667 times)

paranoidandroid · « **Reply #60 on:** November 05, 2010, 01:02:59 AM »

Thanks for the help guys. I tried gassing with dry HCL and no matter how many times I dry the solvents with MGSO4 I don't see any precipitate. The salt comes out of the solution but as an oily substance which I presume to be an H2O contaminated salt. Method of gassing was HCL/NaCL + H2SO4. The oily substance was tested with Marquis with good results. I have tried DCM, Toluene, IPA and different mixtures to no avail. Any ideas?

lugh · « **Reply #61 on:** November 05, 2010, 01:58:38 AM »

You need to use some sort of purification, perhaps this old Hive thread will give you some ideas:

Newbee Forum

   Posts 1 - 11 of 11         Subject: mdma.hcl direct from toluene


        food
(Newbee)
02-12-03 20:41
No 407129
                  mdma.hcl direct from toluene

I heard that 'bob' was dribbling 35% HCL directly into dry toluene mdma freebase solution. Of all the posts that I've looked at only a small minority mentioned proceeding this way. There must be a reason, I thought. Apparently bob has a dish of really white end-product. When I heard about this I figured I'd see what I could find out about this.

--
food



        VinnyC
(One Man Show)
02-12-03 21:24
No 407142
                  The 35% HCL has h20 of course, which is not...

The 35% HCL has h20 of course, which is not miscible with the toluene. You still have to deal with seperation...

Gassing dry hcl would be wiser...

Cheers...
"This is bat country..." Fear & Loathing



        Antibody2
(Bee without a Title)
02-13-03 01:55
No 407234
                  its more of a ghetto way of crystallizing, if...

its more of a ghetto way of crystallizing, if you stir up the toluene/HCl, it will convert the freebase into a salt which then disolves in the water layer, you seperate the water layer and evaporate to get the salt, thats all.
i antibody2, hereby dub this thread a temporary couch



        abacus
(Hive Bee)
02-14-03 06:23
No 407648
                  But brown

Its possible , but if you do it that way, you will probably get brown crystals which can't be cleaned up unless you basify and re-vacuum distill the freebase IME.

But you know you should vacuum distill the freebase before anyway? after that, there is NO substitute for gassing IMO



        SiLiCoN7
(Hive Bee)
02-14-03 13:37
No 407722
                  Wet Extraction --- it works....

An extension on what antibody2 said, and yes, probably the getto style method.... But it works.....(just read the A/B sticky thread)

Swim tried just adding 35% HCL, it makes that solution too acid, it can make your toluene go pink. and it won't form crystals unless you evap all that h2o..

Anyhow, Just mix 20mls H2o and 5mls HCL per 20 gr honey that you expect then add that to your sep funnel with tol/freebase. Shake then seperate the water/acid layer. (it will be on the bottom if using toluene). Repeate this three or four times to get all the goodies, then evaporate the combined water acid extractions on a steam bath and watch the crystals form. (when the very first crystals start to form you can add a little acetone to help it cyrstalize)
When they are fully crystalized, dry and cool, pour about 200mls freezer cold acetone on to the plate you evaporated the h2o in and stir around for a minute or so and break up the crystals to clean them. Then pour the acetone off and leave the acetone 'wet' crystals to dry under a light.

Some will say that this is a cude method for making crystals. But it is by far the easyist way to do it.
You can repeat the acetone wash if your shit is really dirty.
Use a pyrex plate with steep sides sitting on top of a steel pot that the plate sits in snugly, for a steam bath.

I hope this helps you, I firmly believe in gassing if you have the setup and knowledge,(it gives you snow white powder) but it can be a pain in the butt. For the first few times try the wet extraction method to make sure you get all your honey...

Good luck...
the 21st of the 12th 2012......



        food
(Newbee)
02-14-03 19:15
No 407811
                  short cuts
Thanks as usual for input.

I had thought that I'd hear some overriding reason why this was a no-no. I am talking about someone else in my question above. When I am still learning new skills I pick out someone of demonstrated competence and do what they recomend. Go by the book. Because of the research that I did into this I didn't think it was viable for one reason or another. One down side is that without gradually changing and monitoring the ph of added dH2O, you are firing blind I guess.
However I did see the material that bob had harvested from his test batch; it was way white, better looking than what he'd arrived at with more orthodox methods. Don't know if he'd achieve this consistently; I told him to lay off until word got back. ta
--
food



        baalchemist
(Chef d'Equippe)
02-15-03 18:10
No 408163
                  "Some will say that this is a cude method

"Some will say that this is a cude method for making crystals. But it is by far the easyist way to do it."

Gassing is the easiest method by far, using hcl/h2o is just the 'other way' to a HcL salt and requires a bit more patience & time to recover it. It certainly isnt a crude methodology, just one of the basics like an A/B extraction.

GODISNOWHERE
Shoot Narcs, Not Drugs



        Yachaj
(Hive Bee)
02-18-03 23:34
No 409547
                  ALternative to gassing?

After mixing the MDMA freebase in toluene with 35 percent HCl and removal of the upper (toluene) layer, it may be useful to add a splash of acetone prior to evaporation. Perhaps you get not-brown crystals in this way. But this is just a thought experiment. No idea if it works.

But if you have come this far (the freebase) then why take the risk of spoilage. Just gassit!
bibliopharmacophile



        slick14
(Stranger)
03-03-03 22:02
No 413403
                  it works well

when you add the HCl to the toluene and shake it you will get a red oil to fall out get that on to a evap. dish and allow it to dry (not all the way dry) then pour dried acetone over it and then run it through a coffee filter and you have white crystals! bee sure to use plenty of acetone!



        Rhodium
(Chief Bee)
03-04-03 02:57
No 413504
                  Proper purification!

That was one of the suckiest MDMA Hydrochloride preparations I have seen. Can you imagine how much impurities you have left inside the crystals, which you can't see, as well as those impurities which are not strongly colored? What you are doing is comparable to using lots of deodorant and shaving your head instead of showering and washing your hair...

You MUST either distill your MDMA freebase or recrystallize your final product (slowly and properly, not just dissolving it and then "crash" it out) to isolate a product fit for human consuption, and people who take pride in their craft should really do both steps.

"But it'll lower my yield" someone whines... Yes - it is true that the crystals you get after this purification will weigh less than if you didn't, but that is because you have removed everything that isn't MDMA.HCl from it.

If you want to squeeze every last milligram out of your batch, evaporate the solvent you used for recrystallization, dissolve the residue in some water, basify with NaOH and extract with an np solvent and throw what you got back into the distilling flask next time you are distilling MDMA freebase.



        hCiLdOdUeDn
(Hive Addict)
03-04-03 05:52
No 413551
                  Excellently explained.

Yes. Exactly. Thats what I am talking about.

The crystals from undistilled freebase is way nastier than the crystals from distilled freebase. You will be suprised by the bio-essay.
Chemistry is hard to learn, but its worth it.

Distillation of the free base is needed for best results

Sedit · « **Reply #62 on:** November 05, 2010, 02:30:34 AM »

Quote from: paranoidandroid on November 05, 2010, 01:02:59 AM

Thanks for the help guys. I tried gassing with dry HCL and no matter how many times I dry the solvents with MGSO4 I don't see any precipitate. The salt comes out of the solution but as an oily substance which I presume to be an H2O contaminated salt. Method of gassing was HCL/NaCL + H2SO4. The oily substance was tested with Marquis with good results. I have tried DCM, Toluene, IPA and different mixtures to no avail. Any ideas?

Titrate the NP with HCl and extract into water. Toss(set aside) the NP and evaporate the water to yeild crap.Wash with a non polar. Now basify and run this thru an A/B in which you could gas. The "crystals" will be fluffy and white but taking post reaction mixture and gassing like you can do with amphetamines does not appear to work in this case, so I have heard, It just produces the exact thing you spoke of over and over again for no appearent reason.

Extract your shit with water and work from there, end of story.

Author Topic: Bromosafrole success with PTC - Jon's method does NOT work ! (Read 1667 times)

paranoidandroid

Re: Bromosafrole success with PTC - Jon's method does NOT work !

lugh

Re: Bromosafrole success with PTC - Jon's method does NOT work !

Sedit

Re: Bromosafrole success with PTC - Jon's method does NOT work !