place (Stranger)
02-22-04 11:46
No 490418
      Ephedrine form ephedra with only using methanol?     

Hi there.

In ../rhodium /ephedra.html they talking about using ephedrine from ephedra only prepared with a methanol wash.


Approximately 425 grams of ground ephedra plant material was washed three times with methanol. The methanol washings were collected and allowed to evaporate to produce a greenish-brown tar-like substance. To this material was added 250 mL of a 57% solution of hydriodic acid and 9.5 grams of red phosphorus in a 1000 mL round-bottom flask..




Will it be posseble to use the same "greenish-brown tar-like substance" in Placebo's meth Synthesise?

Maybie wash the "greenish-brown tar-like substance" with some cold acetone before useing it. And make 2 recrystallisation at the end.

rgs,

place smile


Flipside
 
 
 
 
    unionpacific
(Hive Bee)
02-22-04 16:25
No 490474
      the green tar will be a mixture of a bunch of...     

the green tar will be a mixture of a bunch of things norephedrine, ephedrine and alot of other stuff you don't want

cold acetone washes will not be enough to give you clean ephedrine, distilling is the preferred route

a ton of info about this on TFSE

There is a thin line between genius and insane
 
 
 
 
    biotechdude
(Hive Bee)
02-22-04 16:48
No 490479
      yes, but low yields     

Will it be posseble to use the same "greenish-brown tar-like substance" in Placebo's meth Synthesise?

It will produce meth.  Yields will be very low.  Workup will be difficult.

Placebo's writeup ../rhodium /meth.rp.html suggests the the use of steam distilling, are u planning on doing this?

If so, the EASIEST way to obtain decent results using plant is to powder 100g 8% plant (or the best % plant u can get), base with NaOH solution to ~700mL, heat to 95`C and bubble steam through from an external source.  Collect 2ltrs of distillate, pH to 6 and evap the water.  Nice white salts...

OR if NOT using steam...
Maybie wash the "greenish-brown tar-like substance" with some cold acetone before useing it. And make 2 recrystallisation at the end.

This wont achieve much, and further wont be possible. How can u RECRYSTALISE the greenish tar like substance?  Mmmm...

At the point u have the green tar, i would recommend an a/b.  However keep in mind that some constituents of the plant are soluble in methanol AND your NP solvent (which you hope would only contain the freebases).  But still a HUGE improvement from the crude methanol extract.

Lastly, the alkaloids you extract from the plant are a mix of structural and chiral derivatives; namely pseudoephedrine, ephedrine, norephedrine etc etc.  AND not ALL will reduce to methamphetamine.  SO your yields will naturally be lower to start with.  Plus if u are using DIRTY feed stock; your yields will suffer even more...

Your call.

Fuck, i need to put all this into a digest or something...
 
 
 
 
    place
(Stranger)
02-23-04 02:58
No 490568
      2 recrystaillation was ment to be made at the...     

2 recrystaillation was ment to be made at the end of the meth-synth. and not with the green tar.

But it seems like SWIM will have to do a strem destil. if SWIM want pure ephedrine from ephedra.

Thank you for your help smile

rgs, place

Flipside
 
 
 
 
    auntyjack
(Hive Bee)
02-23-04 09:08
No 490609
      here's what i reckon     

i;ve seen this method done twice and it produces a very nice drug indeed. as you would have read in that article, the variety of alkaloids reduce down to a coctail of amphetamines and the people i know who tried it say it is lovely.
placebo's method will work on the sludge but you must use a large amount of rp & iodine. you can either work up the sludge to reduce the amount of reagents you use or just use the sludge. you're much better off using dwarfers steaming method but if you don't mind fucking around a bit here's what i've seen done:
.......so, make a METHANOL EXTRACTION...i highly recomend using a percolation setup; a condenser on a flask that drips the methanol through a tube filled with ephedra...make the tube so that the methanol drips out the bottom at roughly the same rate as it is being dripped into the top so that the plant matter is continuously submerged in solvent...this takes a bit of farting around but is well worth the trouble due to the efficiency of the technique; you can use one tenth of the amount of solvent that it takes to do a normal wash...
.......maybe then WASH THE EXTRACT WITH WATER; powder the extract and then put it in boiling or near boiling water(95 C will do)and stir the crap out of it. you're going to want to distill this water to recover the small amount of ephedrine that disolved so don't use too much water unless you like twiddling your thumbs alot. now put the water/extract in the freezer until it is nice and cold (4 C should do)...now make a sand filter(best fucking filters in the world) get some sand and wash the fuck out of it with boiling water until the water runs clear. you can use tap water as long as you use distilled water for the last rinse. then stick the sand in a plastic bottle with the top cut off and holes punched into the bottom or anything like that...you'll work it out...then filter the cold sludgy mess and collect the water..next, scrape the mud out of the filter taking any sand that looks like it has solids in it and repeat the water wash if you feel like it...remember that the mud has most of the goodies and we are trying to wash crap from it...
CLEAN THE DISTILLED WASH WATER WITH NP SOLVENTS;i'm assuming you know what to do here so i won't elaborate but bear in mind that a np wash is not entirely necessary if you are only trying to reduce the bulk of the initial extract and also this is where you come across emulsions like you've never seen(emulsions are easily broken through heating, filtering{allways use a sand filter} or a combination of both...geezmiester has some good advice for emulsions)
.......DISTILL THE WASH WATER; if you use a percolator then you can just replace the tube full of plant matter with a cup or beaker to collect the drips or you can of course use more conventional distillation methods...now titrate the distilled wash water to an acidic condition (roughly ph 5 but utfse as you don't want to be as rough as the guys i've seen do this)and evaporate...you will end up with an orangy sort of stuff that can be scraped off the evap dish with a razor...
.......EXTRACT ALKALOIDS FROM THE MUD; ok, now get your mud from the filter plus the bit of sand under the mud that contains solids(the sand will be darkened under the mud so get it all) and mix it thoroughly with a little water...once mixed as much as possible, add a bit more water(again, amounts are in relationship to how much water you could be bothered evaporating and how much alkaloid you reckon is in your mud...hmmm...utfe)and again, titrate to an acidic condition. the alkaloids are now entering the water...time and motion help here...shake the living fuck out of it and let it sit around for a while. now, you can wash with a non polar solvent which is more desirable with this mud extract than the distilled wash water because the mud extract will contain more shit...again i assume you know how to wash this water with a np solvent, and again YOU WILL GET EMULSIONS FROM HELL!!!...BUT DON'T DESPAIR...emulsions WILL BE BROKEN by heating/filtering, i assure you...so, washed or not, evap the water, collect the precipitate, powder, add to your other precipitate from the distilled wash water and you are ready to rock and roll with a much less bulky extract.....BUT!!!!(now this is important) your yields might be better if you don't frigg around with the initial methanol extract...think about it...all the losses in the work up of the extract could be avoided if you just react the raw extract and save all your working up of the alkaloids once you have turned them into amphetamines...i'm not sure about this one but i'll put it to the guys i know who do this and see what they come up with...(i tried to talk the crazy fools out of doing something so illegal and dangerous but they wouldn't listen!)...

anyway, have fun...bye for now,     
                               aunty jack
PS you will get emulsions in your work up of the reaction fluid so again i cannot stress too much the importance of sand filters...

no...i'm a bloke
 
 
 
 
    place
(Stranger)
02-23-04 11:58
No 490638
      Okay :) SWIM think he is dropping the idea...     

Okay :)

SWIM think he is dropping the idea with methanol crazy because of what biotechdude said and go for damp destil. insted. Maybie just for fun SWIM will try auntyjack methode in a nano reaction smile


@biotechdude: eg. 500g 8% ephedra plant boiled for 45mins. in dH2O water with pH 1-2. Filter and made pH up to 14 with NaOH. Ammount of dH2o 2l to 500g? There after damp destil. and pH to 6 and evap the water. Would that work?

Rgs, place  smile

Flipside
 
 
 
 
    dwarfer
(esoteric)
02-23-04 15:13
No 490676
      try this     

Post 488247 (dwarfer: "The DwarJet: a superheated steam extractor", Stimulants)


You can replace the hose with a flask with a two holed stopper.  ONe with a tube that goes under the liquid level.

If the stuff is prone to foaming, put another similar flask in series: the foam will have to REAlly b intense to fill it as well.  I've never had to use more than one, but if needed, several in line could be provided (up to the size of your P/C) to contain 'foam".

Meanwhile, productivity is undiminished. (It's all just
additional volume kept at the raised temp of the PC
cavity, with hot steam passing thru with alkaloids..)

PS: elevate the flasks from the bottom so they do not
float, or weight them.

PSS: ghetto flask weights that fit around the necks can be made with those silly kid's plastic rings avialable for $0.25
at your thrift store.  Drill a hole, pour in lead shot, epoxy closed  ... viola
 cool



dwarfer
 
 
 
 
    dwarfer
(esoteric)
02-23-04 15:15
No 490677
      opinion as regards final product     

really, it's better.  more gentle and more strong
at the same time.

dwarfer
 
 
 
 
    auntyjack
(Hive Bee)
02-23-04 15:52
No 490683
      hey dwarfer     

..."really, it's better.  more gentle and more strong
at the same time."...

would you be able to clarify that last statement a little.. or am i just a bit foggy and need to go to bed?

no...i'm a bloke
 
 
 
 
    dwarfer
(esoteric)
02-23-04 16:02
No 490686
      you gotta try it     

it doesn't hammer you or give you the grindies,
but you are totally tweaded, and when it goes away,
it doesn't leave you all depressed.

OK OK come to thik of it this was electrochemical stuff,
too: so ...     ??

<<disregard..  ":<)

dwarfer
 
 
 
 
    auntyjack
(Hive Bee)
02-23-04 18:59
No 490715
      i see     

this has been the reaction from people to the meth,amphet,nn-dimethyl coctail as well...very smooth..do you know whether any of the other molecules come over with the steam apart from ephedrine?

no...i'm a bloke
 
 
 
 
    dwarfer
(esoteric)
02-23-04 19:19
No 490719
      other steamed overs from ephedra.     

Based on the fact that the crystalline mass is "mixed"
in both the base and salt modes,
there is no question that there are other species present,
 but which I could not tell you.

I would think any of the similar sized stereoisomer +- up down left right in out alkaloids would come bombing over.

<<<< has acquired a melt point apparatus device for $1,150 off it's usual price from an un-named on-line bidder,


and hopefully in the future may be able to report with
more specific information.tongue

dwarfer
 
 
 
 
    biotechdude
(Hive Bee)
02-23-04 23:33
No 490757
      comments     

@biotechdude: eg. 500g 8% ephedra plant boiled for 45mins. in dH2O water with pH 1-2. Filter and made pH up to 14 with NaOH. Ammount of dH2o 2l to 500g? There after damp destil. and pH to 6 and evap the water. Would that work?

That sounds much better.  It would be a good way to start and gain experience before venturing into the land of Dwarjet.

To tweak your procedure, i would put your plant in a blender (better with dry ice) to make it nice and powdered to increase surface area that releases the goodies. 

Then not boil but put in one of those cheap ceramic (no rust!) slow cookers; that simmer at about ~95`C.  That way u can "Set it and forget it!" (like a Ware LWR!).  Then pour off/squeeze the acid solution using a pillow case or fine mesh (which will contain the near-dry squeezed plant)

Then, raise the pH using NaOH soltion slowly using lots of stirring.  Cos it generates ALOT of heat which can fry the alkaloids (learnt that one the hard way..)

Then steam distill.  The ammount of collected distillate required depends on many variables.  Eg the ammount of goodies, the temp of the soltuion, the temp of the steam (eg superheated) and the efficiency of your condenser.

So Swix's advise would be to collect 2ltrs.  Then separately collect 1ltr portions until you're bored or the distillate's taste isn't as strong and pH not as high.  Then pH to 6 and evap each portion separately.  That way u can work out how much distillate should be collected (or worth collecting based on time and effort required)
 
 
 
 
    place
(Stranger)
02-24-04 07:16
No 490805
      Thank you for your advices, biotechdude.     

Thank you for your advices, biotechdude.

Why is it the all for you only pH down to 6-7 in anything you do? Why not down to pH 1-2? I have woundered about that many times. ?

rgs, place

Flipside
 
 
 
 
    biotechdude
(Hive Bee)
02-24-04 17:17
No 490903
      pH 6 does the job     

Cos all the alkaloids are converted into their salt by the time pH 6 is reached.  Adding more acid would only run the risk of producing contaminant salt and a yucky taste.  You can pH to 1 and possibly have no difference, but its not RECOMMENDED.