Highest yeilds thanks to MeNH2

[scram]

Here is the deal; swim knows that this would work, in theory of course and today has a big smile about it because the yields produced are the biggest ever for the smallest amount of undistilled ketone using the al/hg. So swim is exhuberant and wanted to share this dream as he knows it will work even on that undistilled shit:

12g Al
31 ml 40% MeAm
48ml dirty ketone matrix (sg 1.154)

Now normally swim had to use ~105ml of this ketone to get this yield but in this he would use 48ml. Also, never knowing the purity of his ketone since undistilled, he always takes a random guess at his purity to be somewhere between 30% and hopefully up to 66% and shoots the molar ratios accordingly for MeAm/Ketone  Ketone/Al hoping that if he does the upper limit that it will give him some indication of the amount of ketone he actually had. Well, I don't know if its simply because less al is used to limit losses of goodies during the washes or if MeAm produces way better molar yields than Nitro, or maybe the ketone he had this time was way higher than all other times done before when using Nitro. I seriously doubt the ketone was any different this time In either both cases of Nitro and Meam the upper limits of nitro and al was put in to max out the yeilds. However, Meam produces way higher yields than nitro.
   The reaction was allowed to run very hot with no external heating, I was surpised to find out how much MeAm heats up a reaction and sustains the heat in it. A mock condenser was made using an elongated large party ballon with a small hole cut out in the other end. This was fit over the sep funnel stopcock and securly fastend above the stopcock with rubber bands. The mouth end of the balloon went over the top end of the tool-mouth flask. Was happens he is the reation can be monitored by watching the balloon expand with gas and kept under slight pressure. Just make sure the balloon doesn't get too big. Yes, it does condense back. It generated its own heat for ~1.5 hours and external heat, high heat was added for ~6 hours and low heat 6 more and last 6 hours no heat (18 hours reaction time). The final product will in theory result to 26.2 grams. Unbelievable for swim on only 48ml crude ketone. I hope my supplier continues to keep swim well stocked with this fun liquid because it blows nitro away. Osmium,you are very right when you said yields are high with this stuff. This shit rocks, fuck nitro!

[hCiLdOdUeDn]

Yes, i too agree that methylamine may bee better but it is harder to acquire. I dont want to make it (cant stand the smell). Nitromethane is the perfect chemical for OTC bees. Fuck yields now...dont bee greedy. The risk is just not worth it. 10grams of MDMA.HCL from 100ml ketone is just as good to me as 100grams from 100mL ketone.


hcildoduedn

[terbium]

I dont want to make it (cant stand the smell).
There is no smell! Not if you have any lab glassware at all. All you need for an odorless synth is an rb flask, claissen adapter, thermo adapter and condenser. The only way that there would be any smell is if you try to use that silly preparation that involves cooking in open pots.

10grams of MDMA.HCL from 100ml ketone is just as good to me as 100grams from 100mL ketone.
I will try to refrain from comment on this.

[placebo]

I agree, I saw someone make a kilo in about 4 hours no mess, no smell using the vacuum method on Rhodium's page and yielded exactly whay he said it would.

[Chromic]

Are you sure you got all MeNH2 from the vacuum method--without recrystallization from the NH4Cl? I really don't believe the yields...

[hCiLdOdUeDn]

terbium-if swihc actually tried to make methylamine.hcl in his distillation apparatus and it worked he would probably go with that as the reduction of mdp2p to mdma looks easier. Swihc has no experience in trying the reduction a la osmium so that is why he does agree with it. In all reality if he did make methylamine and it worked he would use this method as the yields are higher.

But since swihc has only had experience with al/hg nitromethane reduction he knows its validity and he knows it will not fail him. He does not care about yields, but nonetheless he gets an average of %50 yield from mdp2p-->mdma freebase.

You may have experience with both methods, and you choose the osmium reduction better. But swihc must remain hidden in the clouds and that means he must stay OTC.

I just wanted to be on even terms with ya!
hcildoduedn

[Chromic]

I'm a fellow OTC buff, seldom ever venturing to a chem store (unless I have to).

Methylamine is OTC, hydrochloric acid and hexamine are easily located at hardware stores and army surplus stores, respectively.

[terbium]

Are you sure you got all MeNH2 from the vacuum method--without recrystallization from the NH4Cl? I really don't believe the yields...
I have always been very skeptical of the vacuum method. That vacuum method seems to propose that reaction temperature doesn't matter. Some people, to try to justify this, mumble about LeChatelier's principal, as if this is a purely ionic reaction. I find all of this hard to believe.

[placebo]

It was recrystalised several times with ethanol

[terbium]

It was recrystalised several times with ethanol
What was the reaction temperature? Or are you of the belief that this is irrelevant?

[hellman]

My self too beng a OTC "buff", I see alot of excitement in the field of increasing yields using UNDISTILLED KETONE,
This has a lot of potential, geting rid of the time fucking around with vacuum distalltion is a prefereably progresive step,.(possibly enivitable)

-It's all about time,
If the manufacture was legal, then I too would give a fuck about labware,I would buy the finest scientific labware known to man, but with all the associated risks included, and not exactly otc, we could use alternatives.
-that could be your marketing point, to try and slide our perceptions over to being more OTC,.- the risks, oh the risks,
Manufacture of MDMA.HCL with out distillation?

[oh, no, of course it can't be done,]
I don't believe that for a second,
I mean I steam distilled ketone, loved it, but the demand or trust of this kind of info is not needed,.why is that,
because we can live with our percieved risks,

I cannot,.

- When you think about it,
If are currently getting say 20-50% yields from safrol to MDMA currently, without using distillation, [and only a handfull of experimenters], then that is proof enough that
it is worth it,-
I  mean 3 weeks in a shed, making 10 kilos, is a lot of time at the pump,.
And the neglible cost of the safrole, makes the argument closed, .
Could you all imagine that, someone soon will post a method that starts with something like 10 kg of saasafass, and 1  or 3 days later, you safe.- no distilation whatesoever,.
And so what you used twice as much sassafras and a few other cheaply priced precursors,.

Really, a seperate thread or forum on OTC only PREPS would be good,
For us, where we can assmble our fragments of success in this method, and win,
I sincerely look forward to that post,.

-People are fickle, we're a mess of many too many contrainst, limits, and other exciting stuff ,limiting the possible,
be careful what you believe, we a purests, we are pesimists, we know only what we know,
But in truth that has nothing to do with what can be done, with all these limits stripped,.

We are a direct result here, of what couldn't be done,.
Most thigs we do hear, we not possible 12 months ago,
You will see that Perfect Quality crystal MDMA can be obtained without any distillation, we are just not ready yet, becuae we simply the  motivation is not there,


I am all for this work, excellent work scram
I am sure many. many bees would like a nice write up
of your most reliable-todate- proceedure using your o2 wacker, all clean-up and amination details,.
Fuckin' excellent,.
IQ is the rate of logic, as Wisdom increases logic, fear & compromise decrease to reveal objectivity

[chilly_willy]

MeAm is great if its pure and you personally know the individual reaction characteristics of the BS/Osmium method.  Buying the stuff just doesn't seem smart.  Making the crap with the p-form/Nh4Cl method is cheap and clean if u go slow and vent.
The hex route can be tricky leaving residual acid and who knows what in the final product. After some dude tried this, is was somewhat obvious the substance was useless. Maybe it was just the guy.  ::For the Para-:: You really cant just let it x-talize hot. Always use vac.. never go over 107!! Get rid of Nh4Cl.. Extract with hot MeOH..reduce gently.  Freeeeeze. Separate the clear hygroscopic crystals. Use vac filter with saran wrap dam.. Seal immediately over CaCl...evap more meoh (low heat)- then add a *little* more MeOH- freeeeze, and filter another batch of crystals.  You may do this a third time but it can become time consuming. Dispose of the yellow waste filtrate.
Rhodiums yields can easily be achieved with multiple recrystallizations, and diligent temp. monitoring.  IMHO- For OTC bees.. stick with Nitro.  It is much cleaner, and quicker.  Not to bash the BS method..but: if the MeAm/Ketone/Al used is not "right"/pure 90% of the time a minimal amount of a mysterious red oil will always come through-  and taints the x-tals a weird champagne color.  Im no expert so feel free to expand reasons for this. No doubt the product is excellent with an Acetone wash..but usually for most purity is more important...

-

[Osmium]

If are currently getting say 20-50% yields from safrol to MDMA currently, without using distillation, [and only a handfull of experimenters], then that is proof enough that
it is worth it,-
I  mean 3 weeks in a shed, making 10 kilos, is a lot of time at the pump,.
And the neglible cost of the safrole, makes the argument closed, .
Could you all imagine that, someone soon will post a method that starts with something like 10 kg of saasafass, and 1  or 3 days later, you safe.- no distilation whatesoever,.
And so what you used twice as much sassafras and a few other cheaply priced precursors,.

Well, I got a surprise for you. For many bees the time of cheap unlimited safrole are long over.
I consider safrole to be the limiting reagent. I treat it as if it was worth its weight in gold. Because I can get all other chems rather easily and in pretty much unlimited amounts (compared to safrole).
Sure, you can make honey without a single distillation. Been there done that, and the yield wasn't that bad either (but lower than properly purified stuff).
But the purity you will achieve this way sucks. Your quality is directly proportional to the SQUARE of the time you invest! Don't encourage newbees to go the 'easy' way, because it is NOT easier!
I'm not fat just horizontally disproportionate.

[RoundBottom]

if you can't do this...

Post 323193

(RoundBottom: "Chromic’s Methylamine.HCl", Methods Discourse) then you shouldn't be here.  the MeAm from this method is 100% funtional in the Os/BS amination. 
my mouth tastes like burning.

[muium]

Yes, MeAm is the best. The Al/Hg/nitro is fine for getting your feet wet and gaining lab experience, but if you don't eventually move to MeAm, you will end up wasting so much time and chemicals in the long run.

Making it is easy, cheap, and OTC. Getting it clean and dry is a bit more time consuming, and can be frustrating if you live in a swamp (due to the hygroscopicity) but isn't rocket science or anything. And if you spent a week or so working on it, you could easily build a massive stockpile.

And once you have MeAm, you have many other options for reductive amination, not just Al/Hg. And you can usually process about 10 times as much ketone in the same flask you used to use for Al/Hg/nitro runs! I'll do 1 big reaction over 10 small ones any day!

I consider safrole to be the limiting reagent. I treat it as if it was worth its weight in gold.

Your first statement is very true, but I don't know about the "worth its weight in gold" part. I've done some calculations (using values from my part of the world) and would say its worth more like 10 times its weight in

And on a separate note:
Is chilly_willy as cool as frost? Or maybe ChemReack finally put out the fire from his last flaming and is now chillin' with a new name?

[Chromic]

I think ChemReack's reputation was pretty much shot with the whole narc thing... but for the record, he certainly wasn't a narc and he did help SWIC out some.

[placebo]

The batch I saw being made was done as on Rhodium's page to the letter. No genius here, just follow directions well and yeild was spot on with expectation.

[scram]

"If the manufacture was legal, then I too would give a fuck about labware,I would buy the finest scientific labware known to man"

...Yeah like buying Quartz type glass boiling flasks for the al/hg. I also realize that there has been exagerated information on the Hive too. This is why I decided to post any let downs in yields as well. This sight is all about posting the range of results that can happen. And I think posting just your high yields gives everyone a false impression for their prospective runs. Therefore swim is going to post a followup reaction that had "let down" yields using MeAm with all the specs for any bee who is interested in numbers:

61 ml undistilled ketone
18 grams al
50 ml 40% MeAm
~300ml MeOH
~140 mg HgCL2 (scale only measures 0.1)
Amalgamated 20 minutes, loaded in 13ml MeAm and dripped ketone/remaining MeAm in 100ml MeOH over 20-25 minutes.
Resulting yield much lower than before 16.2g. But if these crystals are recrystalized it would be more like 14g. Strong enough at 140mg. I think the ketone was not as much in this last wacker and resulted in the lower yields. This yield is still slightly higher than the same measurements of ketone using Nitro in several past runs (maybe ~10% higher). The density of the ketone this time was ~1.17. Higher than the last batch, but I guess isosafrole must be above safrole and threw me off when I just assumed that it would be just as good yield if not better than the first post. Also the successful wacker with the high yields ran extremely hot at a low pressure (less than 25 psi) for at least 1 hour during the apex of the 02 take up (Dont run pop bottles past 25 psi when very hot). Swim is going concentrate more on running the wacker hot instead of being so worried about it being over 40 psi in the next runs and see if yields are more consistent.

[scram]

77ml oil (not distilled/post 02 wacker) d = 1.189 to 1.190
11.2 g al (HD foil)
30 g 40% Hooch (d = 0.902)
68 mg Hg

Amalgamated al for 25 minutes in about 450 - 500 ml MeOH until modest bubbling and slight warmth. Dumped in 15 grams 40% Hooch in and started dripping ketone + 14 g Hooch + 175ml MeOH all in sep funnel. Reaction became exothermic within 7 minutes of dumping initial Hooch in. Several kilos of ice was use to minimalize vapour loss. When dripping was finished about 22 - 26 minutes later the reaction was running very hot and stirring very  vigorously. Heat was applied to ~ 55c for the next 4 hours. About 2.5 hours after drip. The MeAm smell was a little less evident and 1 g was added making the total hooch content 30 grams. There really was little or no reflux. Only ran it hot. At the 3.75 hour mark heat was turned off and run until amalgam was lukewarm. After 4.5 hours total from ending of drip the solution was slightly warm. Dumped solution into 600 ml 20% NaOH and witnessed solution bubble and turn dark grey/black with oil spots floating on the top and falling to the bottom. Decanted off the oil ~70 ml and  "X-tracted" the remaining amalgam 3x with 300 ml toluene each, making total 900ml toluene. Dumped 70 ml oil and toluene together. Several salt washes were done and extracted amine with Hcl. Drove off some of the water off the extract with heat and a fan. Threw in a pyrex 500ml bowel and allowed to crystalize over 3 hours. Added 1 liter (un-dried) acetone over the next 4 hours until crystals came out white. Total Yield 43.5 grams. And this was without even keeping the decanted acetone in the freezer for more than 3 hours. Bioassay @ 125mg was positive. Will report next run later.

[hellman]

Beautiful, your a dream,
thanz for your write up, it is very helpfull,.
more than likely i've missed your o2 wacker write up, I'll search for it now,
well done, read a book today on tsuii, you know, that guy that started this crazy mess, i remember a quote from it saying how it works extremely well with  terminal olefins, making beautiful methyl ketones, it's just great,.

[scram]

Another run done with just a few differences in al/hg time. Also this wacker was run 28 hours instead of 17 on the previous due to cold temps being uncontrollable on the 28 hour run. Pd/cucl2 = 1/4.5 104g alkene/0.82g pdcl2. 95ml Alkene to ~310ml MeOH in a pop bottle at 50 psi down to 30 psi. Total pressure drop between these ranges was 68 psi.

75 ml oil (d=1.175 - 1.176)
11.2 g Al
68 mg Hg
29g 40% hooch + 1 more g added 2 hours after addition (30g)

amalgamated for 25 minutes but amalgamation solvent ~500ml was a litte colder because of ambient temp (~10c)
added 17ml hooch after amalgamated and poured remaing amount into ketone with ~ 175ml MeOH into funnel. Dripped mix in over 25 minutes. Was noticable slower to go exothermic due to ambient temp. additional heat on 2.3 added and stirred full blast. At the 2 hour mark 1 more gram of 40% hooch added. Amalgam ran ~55c. Very little if any reflux drip. Couldn't really see too well into the flask given the opaque flask (from the amalgam). This was intended to run the same time as the previous (4.5 hours). Instead, due to logistical problems it was unable to be run so short. Heat was turned off at the 7 hour mark after drip finished. Ran for another 30 minutes until slightly warm. Dumped grey slurry into 700ml 20% NaOH. But this time no oil fell out. Created an emulsion upon adding toluene probrably because the 20% NaOH was very cold and viscous. Emulsion separated and had to be dealt with using time and patience. 3 extractions totaling 1000ml toluene done over 4 hours. Washed and washed. Acidified with something like 60ml of 31.45% hcl and was still ph 8. Brought it down to 1. Toluene was 5. Cleaned up with acetone (dried this time using 25g MgS04) in 1.1 liter acetone (had about 100ml of toluene added to the acetone too. Resulting yield was 38.5 grams of same goodies as above. MeAm blows the shit out of Nitro. Yields in the part of town have nearly doubled since. Why does this stuff give such bomb-ass yields compared to nitro? I've never had so much. The total of the 2 reactions fill the bottom part of a zip lock bag about 1.5 inches.