Author Topic: NaBH4 is just amazing.  (Read 29674 times)

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cublium

  • Guest
NaBH4 is just amazing.
« on: September 30, 2003, 07:55:00 PM »
Cub ran his first NaBH4 reduction few days ago and found that this reaction is simply amazing.Only the dissolution of methylamine in methanol was bit complicated as methanol had to be constantly cooled during bubbling.Methanol was weighed before and after gassing and about 30 grams of methylamine had been dissolved in methanol.Added 80 grams of ketone(solution turned orange) and prepared an ice bath.Reduction took place in 1 liter round-bottom.Temp was kept below 15C with a bath filled with ice/NH4NO3 and everytime it dropped to 7-8C more borohydride was added which caused foaming and rise in temperature.Total of 14 grams of borohydride was used but when about 9 grams had been already added further addition didn't make temperature rise like it had been(probably all that there was to reduce was already reduced),still that 5 grams was thrown in and left solution to stir for 12 hours at low speed.Next morning cub discovered that colour of solution had turned to bright yellow(it was orange just after addition of ketone to MeOH/MeNH2).Solution was poured to sep funnel and added 1 liter of water and some 100 mls of DCM.Sepped off bottom layer and washed other one with some DCM.DCM and bottom layer was poured together.Evapped DCM to yield about 70 mls of almost colourless liquid with a distictive smell(little like methylamine or isosafrole glycol).Cub has never got such nice freebase from Al/Hg reduction.Freebase was dissolved in 600 mls of xylene and result was a colourless liquid.It was gassed and whoah,just like a toothpaste.Filtered at vacuum and gassed again,same result.Filtered and tested xylene to contain no more freebase(it was acidic).Bright white powder was rxtalled from acetonitrile(1 gr and 7 mls),dried.Yield was 70 grams of white powder that tasted quite bitter.This makes w/w yield nearly 90%,cub has never got such yield and purity with an Al/Hg reduction(w/w yields rarely exceeded 75%).NaBH4 is the shit,cub will never run an Al/Hg again.This was cub's first NaBH4 reduction and results are impressive.
PMK used was 96% pure confirmed by nMR(C13 and something else,sorry,cub knows nearly nothing about analysis,if needed could post some charts with some peaks,dunno how these are called),other 4% was safrole.
Borohydride,methylamine and methanol were all lab grade.
Special thanks to LabTop for posting such nice writeup(check rhodium site).

scram

  • Guest
I was once also amazed by how easy it is to...
« Reply #1 on: October 01, 2003, 04:18:00 AM »
I was once also amazed by how easy it is to clean up the NaBH4 post reaction. It's much less messy and makes little if no emulsion. Even when using  al/hg with Aq. meam and reducing the al down to 1/3 of the nitro reaction, it still is a much cleaner post-clean-up process. Yield was only slightly less than what was achieved with al/hg/meam method.
Does anybody know if adding the aqueous MeAm to the methanol and stirring for 30 minutes with MgS04 actually removes the water in a ratio that keeps the amine in the MeOH? I read on here someone used a drying column with mgs04 + silica gel to remove the water. However I was with the understanding that the water is removed proportionally with the amine into the mgs04. Even Osmium mentioned this some 3 years ago. I did some research on his comment to follow up and it mentioned that mgs04 does indeed have a priority of what it absobs being water first, blah blah, and amines somewhere along the line.

cublium

  • Guest
cub has heard that some add silicagel to rx...
« Reply #2 on: October 01, 2003, 06:20:00 AM »
cub has heard that some add silicagel to rx mix in the beginning so that water would be removed as imine forms.Yet another thing to try,silicagel is very cheap anyway.

technology

  • Guest
(Post deleted by technology)
« Reply #3 on: October 01, 2003, 06:54:00 AM »

cublium

  • Guest
Cub is not saying Al/Hg is bad,when he didn't...
« Reply #4 on: October 01, 2003, 07:03:00 AM »
Cub is not saying Al/Hg is bad,when he didn't have access to borohydride,cub ran some successful Al/Hg's also(45 grams of amine from 60 grams of ketone) but NaBH4 is just so foolproof and very high-yielding at the same time,if you use common sense,it's very hard to fuck up.Al/Hg,on the other hand,is very prone to fuckups,at least in cub's experiences...

technology

  • Guest
How bad of me
« Reply #5 on: October 02, 2003, 02:48:00 AM »
what, so what you are saying moderator who ever you are, you are not allowed to speak your mind/opinion.. how wrong of me.. i am sure people can differ between you rating and mine.. chill out..


Rhodium

  • Guest
Self-rating is to misinform other users
« Reply #6 on: October 02, 2003, 03:34:00 AM »

Our rules

(https://www.the-hive.ws/) reads as follows: "No offending, off-topic, crossposted, misinforming, or insignificant postings."

If you fake a certain rating of your post, then you are per definition posting misinformation, hence you became rated.

May I ask why you erased your post if you were so sure about you behaving properly?

technology

  • Guest
I know the rules Rhod.
« Reply #7 on: October 02, 2003, 06:57:00 AM »
I know the rules Rhod. i did not want to offend anyone and i merely back up my opinion in my other post. Anyhow rhodium i rated it as a good read it was my OPINION not someone elses, therefore what is the problem..

it is not like i rated the post as good read on the original post.. if people cant read between the lines that is there problem..

as all i did was state my opinion which seems to have been neglected..

Tell me rhodium what is the difference if i had suggested it was a good read in my text.. would it be a diff story then? i ask.

Sorry for deleating do not wish to offend? and i still back my self up with a good argument...


peace....no harmful intent meant... just opinion ;)

Rhodium

  • Guest
not quite
« Reply #8 on: October 02, 2003, 05:19:00 PM »
Anyhow rhodium i rated it as a good read it was my OPINION not someone elses, therefore what is the problem.

You didn't say it was in your opinion, you imitated a real rating text, which was very close to a real one.

Anyhow, please continue in PM if you have any further to say, as this is off topic.

cublium

  • Guest
Scale-up was performed.1 kgs of ketone,300-400
« Reply #9 on: October 13, 2003, 11:01:00 PM »
Scale-up was performed.1 kgs of ketone,300-400 grams of methylamine was dissolved in 4 liters of methanol and 100 grams of borohydride was used during reduction.An ice bath with ice/ammonium nitrate was used and it kept temperature within limits just fine.Borohydride was added over 2 hours.Left away to stir for 12 hours.Mix was flooded with water and extracted with 1,5 liter of DCM.DCM evapped to leave 1 kgs of raw base.300 grams of that base was gassed in 3 liters of toluene to yield 256 grams of white amine hydrochloride salt which means cub will get total of around 850 grams of amine salt out of that reaction,nice,nice indeed...
This all proves that NaBH4 is perfect for both large-scale and small-scale MDMA preparation.

Rhodium

  • Guest
66% Yield
« Reply #10 on: October 14, 2003, 02:33:00 PM »
1.00 kg MDP2P (178.2 g/mole) = 5.61 moles
0.85 kg MDMA.HCl (229.7 g/mole) = 3.70 moles

3.70/5.61 = 0.66

=> Yield: 66% (Not stellar, but okay, considering the ease)

cublium

  • Guest
Cub always gets around 85 grams out of 100...
« Reply #11 on: October 14, 2003, 03:52:00 PM »
Cub always gets around 85 grams out of 100 grams of ketone.Maybe ketone he has been using is bit impure.It was made by who knows who and has been standing at room temperature for at least a year.Or maybe silicagel helps.Will try this silicagel stuff in near future.

abuse

  • Guest
This method might be easier and higher ...
« Reply #12 on: October 17, 2003, 12:58:00 AM »
This method might be easier and higher yielding than Al/Hg, but methylamine is not obtained easily. Instead of using MeNH2 (methylamine gas) in this reaction, can one substitute nitromethane as the methylamine source in the same way nitromethane is used in Al/Hg?

UKBEE

  • Guest
nope
« Reply #13 on: October 17, 2003, 01:16:00 AM »
nabh4 doesn't reduce the nitro group..(so you can't do a one pot with nitromethane)

you could always a Al/Hg on nitromethane to make your methylamine first...(pain) but it saves buying it


cublium

  • Guest
In this case methylamine was bought but cub...
« Reply #14 on: October 17, 2003, 05:35:00 AM »
In this case methylamine was bought but cub has also used home-made methylamine with same yields.He has been constantly getting 85% w/w out every time(kilo scale and 100 gr scale)Maybe he should silicagel.Or try to use purer ketone.

armageddon

  • Guest
methylamine via pd/c?
« Reply #15 on: March 24, 2004, 07:45:00 PM »
Has someone tried to make methylamine by reduction of nitromethane with pd/c and ammonium formate? My idea would be to reduce nitromethane with CTH under anhydrous conditions, slowly heat up the rxn mixture and bubble the resulting methylamine gas into aeq. HCl to get the hydrochloride in aequous (stable) solution. By weighing the HCl before and after gassing one could determine the amount obtained. Could this work?

THX A

(by the way - I've just become newbee, thanks!  8) )

Rhodium

  • Guest
Nitromethane -> Methylamine
« Reply #16 on: March 24, 2004, 09:37:00 PM »

armageddon

  • Guest
nitromethane -> methylamine (2nd)
« Reply #17 on: March 25, 2004, 10:33:00 PM »
Seems SWIA should UTFSE a bit more...

anyway:

https://www.thevespiary.org/rhodium/Rhodium/chemistry/cth.nitro2amine.rani-hcooh.html

looks good too for preparing your own methylamine hcl. Raney nickel could be substituted with pd/c easily (SWIM has no raneyNi :) ). But my question is: how would one separate methylamine? solvent extractions at -7°C? Would't bee easy ;) Any suggestions? washing with cold brine and then boil off the desired amine perhaps?

THX a

baalchemist

  • Guest
Whats so difficult about the Al/Hg reaction?
« Reply #18 on: March 27, 2004, 06:53:00 PM »
Whats so difficult about the Al/Hg reaction? The only potential problems/failures are ones caused by the inexperienced persons running it, but that can be the case with any reaction regardless of its seemingly simplistic protocol. A good solid understanding of reaction procedures/details brings that possible failure % down considerably with any reaction. Some bees have shown/proven far better yield %'s via the Al/Hg/nitro in half the time, & Osmiums Al/Hg version brings those yield %'s up even higher yet.


XrLeap

  • Guest
hi SWIM might bee just asking some stupid...
« Reply #19 on: March 27, 2004, 08:43:00 PM »
hi

SWIM might bee just asking some stupid questions....

1) Can SWIM use Methylamine solution in the borohydride reduction method? If yes, can SWIM just add it to the rxn vessel like adding water?

2) If not, can SWIM boil the Methylamine solution to make the gas, as the boiling point is 48°C? It sonds like a bad idea as it has the following hazards "Vapors or gases may ignite at distant ignition sources and flash back.
  Vapor/air mixtures are explosive."


any kind words for the answers would be much appreciated.:)

Edit: 3) And the weight of the Methylamine mentioned in the NaBH4 synthesis is in .hcl or gas?


XrLeap

  • Guest
Thanks mate
« Reply #20 on: March 27, 2004, 09:45:00 PM »
thanks buddy for the reply:)

however, there are some more questions following them, swim is puzzling and doing a lot of reading. swim just can't visualise how to make them happen.....

1)can swim just prepare some methylamine.hcl and add them in sodium hydroxide in a rbf(thus producing methylamine gas)?

2)and the product needed would only bee the gas to dissolve in the rxn vessel(the methanol mixture from NaBH4 reduction method for e)? the other by-products are all not needed, but can swim just add NaOH and methylamine.hcl in the methanol mixture in the rxn vessel?

3)can swim just place the rbf(2 neck) higher that the rxn vessel to pull out the methylamine gas by the differential pressure, as methylamine always drop onto floor?

sorry if these questions sound stoopid.... :-[


XrLeap

  • Guest
arghhh... i really do sound stupid.
« Reply #21 on: March 27, 2004, 09:55:00 PM »
arghhh... i really do sound stupid. the answers to my questions are all here....

Post 443313

(LaBTop: "Hydrous Boro One Pot !  AT LAST!", Methods Discourse)



armageddon

  • Guest
RE: What's so difficult about the Al/Hg reaction?
« Reply #22 on: March 27, 2004, 11:51:00 PM »
Baalchemist: Probably you're right. Perhaps I'm a bit overscared and a sissy, but I strongly disklike working with compounds like HgCl2 in amounts required for medium-scale RXNs. If anything runs out of control (and everyone experiences this now and then), you will have a problem if the rxn didn't take place in a lab fume hood  :o  ;D . And therefore it's not a question of yield but rather security/health issues...  :)  (although borohydride is toxic, too, but mercury-2-chloride is quite a bit more nasty I thought.. Did you know that mercury poisoning causes insanity?)

I absolutely don't doubt that Aluminum Amalgam reductions can produce very high yields at low cost of reagents and short rxn times. But I thought that avoiding the use of toxic compounds (where possible) is good lab practice? :-[  (ok perhaps I'm just too scared, but I just cannot feel safe when I know that there MIGHT be some residual mercury-(whatever) traces at my work space beecause a recent Al/Hg reduction was a bit too exothermic/not enuff ice was at hand :( , lack of experience indeed. Of course this is only fictional and didn't happen at any time.  >:(  >:( )
But It's of course the method of choice for big scaleups!  8)

DeeMtermined: WOW! Looks indeed very beutiful, really sparkling! (hats off)

XrLeap: Nice thread you digged up! Thanx for the info! Will have to do some reading..  ;)

methlab

  • Guest
Hydrous Boro One Pot ! AT LAST!
« Reply #23 on: March 29, 2004, 02:23:00 AM »
Hi! I am very interessted in this method. My question is, has one more detailled infos for aminating MDP2P with NaBH4 using this method? It says "Longer reaction times and 4-5 eq ethylamine should give better yields". So, how long should i run it, and how much methylamine.hcl should i use ? Greetings

Bandil

  • Guest
When using the "wet" amination ...
« Reply #24 on: March 29, 2004, 01:27:00 PM »
When using the "wet" amination scheme, the best yields are usually obtained from using a 1:2.5 ketone to methylamine ratio. Mix the ketone and aq. methylamine in a proper solvent (IPA is fine), cover the mouth of the flask with some foil and stirr it for about one hour at rt.

After one hour you can add the aquous borohydride solution(1:1 ketone:NaBH4 molar ratio is perfect ) dropwise while stirring heavily. Please remember to basify the aquous medium you are using for the borohydride prior to the introduction of the hydride, to avoid decomposition. After addition of the borohydride, the flask is covered with some foil and stirred overnight (a few hours is usually enough, but better safe than sorry).

Then proceed with workup as usuall. Quite an amount of xP2Pol can be salvaged from the non-polar washings, so please do reuse this for other runs. Rhodium has written some good posts on this topic.

regards
Bandil


methlab

  • Guest
Thanx
« Reply #25 on: March 29, 2004, 07:44:00 PM »
thanx for your advice, will try it this weekend.
greetings

baalchemist

  • Guest
Armageddon; Those fears are just normal, and...
« Reply #26 on: March 30, 2004, 11:04:00 AM »
Armageddon; Those fears are just normal, and may subside in time. The reaction needs headroom mainly in order to 'keep it together' safely. The Hg salts are used in minimal amounts(200-300mg's will work in a 100-150g reaction) Big, oversized flasks will give the best returns. Baal had used his 22L for 100g reactions, and with the large amount of available headroom, it could be run at full bore without a worry & return 100g+ in a final yield. Ultimately one needs a comfort level with any reaction method they choose. Regardless, its great to hear about success for anybody using any available method.


ranxerox

  • Guest
Armageddon: If (Al/Hg) runs out of control...
« Reply #27 on: April 01, 2004, 01:14:00 AM »
Armageddon: If (Al/Hg) runs out of control... you will have a problem if the rxn didn't take place in a lab fume hood

First, the "Hot Part" of the Al/Hg only lasts about an hour at most.  If you cannot stay put and watch your reaction for that long, don't do it and find another hobby.

Second, if you do get a runaway reaction, holding chunks of ice to the sides of the rection flask will slow it down enough to avoid an erruption.

I know that there MIGHT be some residual mercury

The elemental mercury will be in the sludge as a small drop.    If you want to be certain of mercury free product, you will have to distill your freebase (after washes, of course).

Baal: Baal had used his 22L for 100g reactions

Are you talking about a nitromethane Al/Hg, or are you missing a 0 there?  A carefully controlled 100g nitromethane Al/Hg can be run in a 5L flask.  A 250g MeAm Al/Hg can be safely run in a 5L flask.  You must really demand a lot of headroom.

silenziox

  • Guest
If you want to be certain of mercury free...
« Reply #28 on: April 01, 2004, 01:28:00 AM »
If you want to be certain of mercury free product, you will have to distill your freebase (after washes, of course).

And If you want to use the patented double-condom-safety(tm), you could make the alpha-lipoate salt with alpha-lipoic acid.. It removes quite efficiently Hg and other heavy metals from your body.


Rhodium

  • Guest
Seriously, don't try that.
« Reply #29 on: April 01, 2004, 02:32:00 AM »
I do not think alpha-lipoic acid will give a suitable salt.


XrLeap

  • Guest
swim is noobee and swim do not like to assume...
« Reply #30 on: July 04, 2004, 12:28:00 AM »
swim is noobee and swim do not like to assume things he does not understand, so, asking a question that might sound stoopid.

can one use methylamine.hcl and add them to the solvent(methanol in this case), will the yield be affected badly, or will there will any yield at all?
in the earlier post stated methylamine, swim is assuming methylamine gas, right, there is methlymine solution so which is the actual used chemical?
in the rhodium site, methylamine.hcl was mentioned could be used, but so far no %yield was reported. can any bee kind enough to share the experience?

thanks


Snakebyte

  • Guest
glassware setup
« Reply #31 on: July 14, 2004, 11:54:00 PM »
What type of glassware do you use for dissolving your methylamine gas into the methanol and how is it set up?  Assume that your reacting methylamine.hcl with NaOH.  I've read the huge scale method using a gas tank and a tank of methylamine(by Labtop?) but I'm asking about smaller quantities with regular glassware.


cublium

  • Guest
It was like pressure equalized addition funnel
« Reply #32 on: July 15, 2004, 05:06:00 PM »
It was like pressure equalized addition funnel on 2 necked RB with other neck connected to tube which lead to chilled methanol.Saturated NaOH solution was dripped into MeAm.HCl and that was about it.Learn to control the apparatus,suckbacks occour if you're not careful(add NaOH solution slowly and don't cut the flow suddenly and stir the mixture constantly).You may want to use wash bottle between apparatus and methanol solution.

r2e3

  • Guest
i cant wait
« Reply #33 on: July 15, 2004, 10:40:00 PM »
i have the cleanest me.hcl and FB - a yield would be good - have such a complicated rig to get rid of water now - free partie this w/e too - be nice to be cuming in my head - tired of all the street shite....... been too long

Snakebyte

  • Guest
another question for cub
« Reply #34 on: July 20, 2004, 12:07:00 AM »
Ok cub, so the tube that carried the gas to the methanol came up through the bottom? or came down through a stopper of a flask with the tube going down to the bottom of the flask or what?  Was there a vent in the flask with the methanol for any built up pressure or does the methylamine get absorbed completely with no increase in pressure?  These may be stupid questions but I'm not familiar with dissolving gas into a solvent.


cublium

  • Guest
Here it is,cub also advises to use flask for...
« Reply #35 on: July 20, 2004, 07:56:00 AM »
Here it is,cub also advises to use flask for methanol and not a beaker,in a beaker it'll fly into atmosphere faster than you can add it.In a flask there will be very small loss and smell.

Chimitant

  • Guest
Wet piece of fabric to trap smell
« Reply #36 on: July 20, 2004, 10:49:00 PM »
Nice drawing Cub! To prevent methyl amine gas escaping you could wrap a wet piece of fabric around the top of the left flask (Even better, use a second wash bottle filled with methanol)


r2e3

  • Guest
and dont forget!
« Reply #37 on: July 21, 2004, 12:18:00 AM »
to have a diffuser to break the gas into nice small bubbles with continuous cooling -ie 4C i have seen - when cool enough - the gas will literally disappear into solution - ie no smell.
the tube in the diagram should have a few holes (25 gauge) -not to many tho and the bottom plugged to enhance the dispersing effect.

OcoteaCymbarum

  • Guest
What about cooling???
« Reply #38 on: July 21, 2004, 03:56:00 AM »
Cublium, do you cool in some way, the tube leading to the methanol?
Or do you use cold methanol in a cold bath, along with cold naoh and meam solution??

Ive never gassed meam but i was under the impression that cold methanol(ex -20 celcius) wouldnt be enough to keep the meam in. I taught that you would need to cool in between the meam and methanol.

Do you know how much dissolves in for how much initially used???
Could the proper setup be that simple??? I have NaBh4 lying around, i feel like trying a reductive amination of that sort on a primary amine and ketone
OC

cublium

  • Guest
Cublium, do you cool in some way, the tube...
« Reply #39 on: July 21, 2004, 10:57:00 AM »
Cublium, do you cool in some way, the tube leading to the methanol?
Or do you use cold methanol in a cold bath, along with cold naoh and meam solution??

Methanol is first prechilled in freezer to -20 C.Then it's gassed some time and temp rises as methylamine dissolves(solvation seems to be exothermic or methylamine itself is hot as it comes from the generator).When temp rises to few degrees C,stop addition,put stopcock on methanol flask and return it to freezer,and so on till right amount has been added(weigh with scale but use a quality scale or it won't show anything useful when liquids are measured,but good scale will show exactly how much has been added).Cub used a small generator consisting of 2 liter flask for methylamine,half liter press eq. addition funnel and 2 liter flask for methylamine and gassed in few hours over 300 grams of gas to 4 liters of methanol to do a 1 kg PMK reaction.He got nearly 900 grams of amine salt out of that one ;D .He gassed 1 liter of methanol at the time and frozed it few times as it got warm during solvation.When 1 liter was gassed,poured it to 10 liter flask which was kept in freezer and proceeded to gas another liter and when all 4 litres were gassed and cooled to -10 or so,ketone was added in 1 portion,no warming was noted and temp stayed same,solution turned to dark orange though.Then started adding borohydride and so on.Total success even though it was cub's just third NaBH4 reduction(former two were good too,over 85% w/w from both).It's very easy reaction,hard to fuck up if you have already some experience on that matter.Let me put it that way:if you succeed in making ketone from safrole,you definitely succeed with NaBH4 reduction in any scale,it's really as easy as i tell it is,i'm sure many bees can confirm that.

OcoteaCymbarum

  • Guest
Thanks for the input
« Reply #40 on: July 21, 2004, 04:47:00 PM »
Thanks cublium, I think I will give your method a try, since it seems to work no problem.
What has always stopped me was the fact that I really wondered about the gas escaping off the Methanol.
Im sure its straigth foward, thanks again!

r2e3

  • Guest
yes
« Reply #41 on: July 21, 2004, 08:56:00 PM »
quality experience vs quantity experience (or maybe a concise recount) good shit all the same

cub - you euro? - so tempted to buy the MeNH but been a bit chicken - so cheap too...


Chimitant

  • Guest
Remember
« Reply #42 on: July 21, 2004, 09:17:00 PM »
Cooling is important when doing this type of reaction. It will give higher yields compared to reactions done at room temperature. I think this can be ascribed to a decrease in formation of 3,4-MD-propan-2-ol at lower temperatures.

Yields mentioned by Cub are confirmed by other bees...


cublium

  • Guest
cub - you euro? - so tempted to buy the MeNH...
« Reply #43 on: July 21, 2004, 09:35:00 PM »
cub - you euro? - so tempted to buy the MeNH but been a bit chicken - so cheap too...

Yes i'm euro and at the moment being charged for MDMA manufacture.MeNH2 is cheap but will sure draw some attention.Cub has used homemade methylamine in NaBH4 reduction too and with same yields as with bought MeNH2.My advice: don't try to buy methylamine
NaBH4 is at least as suspicious as MeNH2 so be careful.

r2e3

  • Guest
thanks
« Reply #44 on: August 04, 2004, 12:16:00 AM »
for the advice - i have all NaBH4 i need to sort myself out but guess will have to resort to yea ol ammonium choride/ formaldehyde or hexamine/HCl synth for MeNH2

sounds like you have this whole process down to a T - if there was a drooling emoticon it would be here  :P

armageddon

  • Guest
my full sympathy to cub..
« Reply #45 on: August 04, 2004, 01:54:00 AM »
Cub: You got busted for MDMA manufacture? Did you buy MeAm40% and NaBH4 from an official chemical trader (maybe even both from the same one?) Anyway, I really feel with you - hope you won't get too much trouble though. (tell'em your several mole scaleups were all intended for your personal home use - and get a GOOD lawyer! Really, being addictive is a good excuse... ::) )

To r2e3: Already have a look at

Post 488683

(Organikum: "For the vindication of Eleusis - Methylamine", Methods Discourse)
Easy MeAm at home...  ;)

(always be prepared for having answers at hand when you're asked about why you came into posession of this and/or that - and I mean fictional, unsuspicious but nevertheless REASONABLE answers.. And if you can't come up with good excuses - store the suspicious compound elsewhere, not in your lab!! And when asked about its whereabout, tell'em you flushed it down the toilet because of health concerns...)

Greetz A


cublium

  • Guest
Methylamine(salt) and borohydride were bought...
« Reply #46 on: August 04, 2004, 09:46:00 AM »
Methylamine(salt) and borohydride were bought by someone cub knows with a false ID.They were both bougth from one company though :o

r2e3

  • Guest
pretense
« Reply #47 on: August 05, 2004, 02:14:00 AM »

DoctorFeelgood

  • Guest
cublium you are my nightmare for today !
« Reply #48 on: August 06, 2004, 12:49:00 AM »
cublium you are my nightmare for today ! i'm living in europe too, sure not very far from you. did they arrest you just for buying a precursor, or did the find some mdma too? buying things like meam salt/gas/solution in europe is very very hot and this was a big mistake. hopefully the laws in your country are less strict than in mine. more than 10g mdma is called a "big amount" here, a guarantee for a couple of months in jail. >= 100g is called a "super big amount" here, which would result in a very long holliday in jail.
i hope that other bees will recognize, that our game is very very hot and illegal. if this would have happened to me in my country, i would not be in freedom anymore (do they have internet in jail???). i think i should clean my house and buy a big bottle of diazepam tomorrow - shit this is also illegal...
best wishes cublium, let my know how much they gave you for your joke.

psytech

  • Guest
NaBH4 is just amazing
« Reply #49 on: August 08, 2004, 03:24:00 AM »
Swim is currently working up a Nabh4 p2p, swim is out of DCM, the only none polar he has is toluene, can he use it as a subsitute?

r2e3

  • Guest
yes
« Reply #50 on: August 08, 2004, 08:21:00 PM »
not quite as a powerful solvent as DCM but should get the job done. check rhodium solvent miscibilty chart. It'll give you a good idea of the polarity of each solvent. DCM is 3.1 and toluene 2.8 off the top of my head

armageddon

  • Guest
..d'oh!
« Reply #51 on: August 08, 2004, 09:05:00 PM »
So, your buddy "SWIM" is making meth at the moment???? Are you crazy, or why do you post about it in this thread? Just after Cub told us about his bitter fate? (in case you didn't know: it's illegal, in all countries of the world..) :(

Anyway: for extracting insoluble, oily substances from aequous salt solutions - why do you think you couldn't use any other non-polar? Their only differences are different polarity/different solubility in water/different density (i.e. top-puller like toluene or bottom-puller like DCM).
Need I say UTFSE?

EDIT Just realized that r2e3 already replied while I was typing...This post is therefore meant as a reply to the one preceeding r2e3's  :) /EDIT

A


r2e3

  • Guest
hehe
« Reply #52 on: August 09, 2004, 10:18:00 PM »

r2e3

  • Guest
apologies
« Reply #53 on: August 10, 2004, 09:21:00 PM »
for a couple meaningless posts. cublium has provided good advice. distracted,sidelined call it what you want.

this post may be insignificant but i have made my penance

cublium

  • Guest
did they arrest you just for buying a ...
« Reply #54 on: August 10, 2004, 09:52:00 PM »
did they arrest you just for buying a precursor, or did the find some mdma too?
It was bit more complicated but yes they got bit less than 1 kg of high purity MDMA.HCl,not from cub but from some people who rat on him and you know the rest.Some prison time is more than likely to come but may also go totally on probation,they did let cub out before the court with no bail and that is a good sign.Oh well,can't give much details,let's see what happens in court and then may discuss longer on that subject.

r2e3

  • Guest
damned rats
« Reply #55 on: August 13, 2004, 08:15:00 PM »
hope it goes well...
always weak links in the chain that save their own butts

as far as i'm concerned - making your own is doing the general population a favour, be nice if all the law makers recognise that.

Clean MDMA is hard come by but it certainly isn't going to do unexpected things and generally cause nasty side effects.

i wish the numb nuts at the top would look at drinking vs MDMA related deaths per year stats.

i read this article where they say if all 'drugs' were reclassified, alcohol would be class A along with smack and crack. Go figure...

Ban alcohol hahahaha - yeah right. :P

OcoteaCymbarum

  • Guest
Should the methanol be stirred?
« Reply #56 on: August 18, 2004, 11:00:00 PM »
I've been reading about MeAm gas generation. I saw a post by sunlight where he mentionned that stirring is better when gassing methanol with MeAm.
Is that the case? I was under the impression it would make it fly off more easily.

Second question: has anyone ever tried the NaBh4 reductions as per LAbtop on Rhodium's site using Ammonium acetate???
What are the yields like? I'm sure they cant be as good as for MDMA. And what about water formed in that reaction? Should the solution be dried with silica??