The Vespiary

The Hive => Chemistry Discourse => Topic started by: dennispeck on October 29, 2002, 09:45:00 PM

Title: MDP2P to MDMA route
Post by: dennispeck on October 29, 2002, 09:45:00 PM
What do the Dutch mean when they say  : "the cold method"  ??
Title: that's a good question
Post by: SPISSHAK on October 29, 2002, 10:10:00 PM
now somebody who's dutch please answer it.
I've always heard that they use catalytic hydrogenation to put ot the multi kilo quantities, they are so famous for.
Title: Actually it means...
Post by: Jackhammer on October 29, 2002, 10:17:00 PM
you perform the reductive amination reaction at temperatures below zero, e.g. in a freezer. I suppose this gives better yields since less reduced MDP2P is formed. Can someone verify this?
Man´s main task in life is to give birth to himself.
Title: That does'nt make sense
Post by: SPISSHAK on October 29, 2002, 10:20:00 PM
I don't think anything will happen at zero centigrate.
Title: Reaction occurs!
Post by: Jackhammer on October 29, 2002, 10:28:00 PM
the reaction goes well at this temperature. If you have the change just try it out. Those MDMA tablets from tha Lowlands do contain MDMA after all  :P

BTW what reaction are you talking about? I´m referring to the reduction with sodium borohydride
Man´s main task in life is to give birth to himself.
Title: I was
Post by: SPISSHAK on October 29, 2002, 10:32:00 PM
Thinking Platium (adam's catalyst) reductive aminations under hydrogen.
I've always heard this was how it's done there, but I May be wrong.
If your talking about sodium borohydride your probably right.
Those people in Holland must have easy access to chemicals.
Title: You´re correct as well
Post by: Jackhammer on October 29, 2002, 11:17:00 PM
I don´t know exact numbers but I think it is definately true that in tha Lowlands the main route to MDMA is reduction with Pt/hydrogen...
Man´s main task in life is to give birth to himself.
Title: Good lord, if I had just cooked up a few kilos of ...
Post by: El_Zorro on October 30, 2002, 02:45:00 AM
Good lord, if I had just cooked up a few kilos of MDMA powder, and it was laying right there in front of me, I don't think I could stop myself from just jumping in it and rolling around, and maybe rubbing it all over my........uhhh....shouldn't this thread be in the General Discourse forum?
Who is that masked man?
Title: No, because it is an interesting question about a ...
Post by: carboxyl on October 30, 2002, 08:16:00 AM
No, because it is an interesting question about a method of production that obviously has worked for the big boys. I'm curious.
The above post is purely fictional. Any resemblance to "real-life" is purely coincidental.
Title: NaBH4 ?
Post by: Sunlight on October 30, 2002, 07:51:00 PM
May be it is the NaBH4 procedure that LabTop gave us. The best yields and low temperature.
Title: NaBH4 route gives exellent yields.
Post by: raffike on October 30, 2002, 08:37:00 PM
NaBH4 route gives exellent yields.Only problem is that NaBH4 is expensive and might not be available for certain bees.Yields w/w go over 100% :) .
Then there's that platinum dioxide(Adams catalyst) method @ 3 atm H pressure with yields w/w in 90's.
Both methods are pretty cold.NaBH4 rxn contents must be kept under 10C,but i can't remember the temp needed in PtO2 method
A friend with speed is a friend indeed
Title: temperature
Post by: Jackhammer on October 30, 2002, 09:57:00 PM
The temperature should be kept around 50 °C when using Pt/H2 if I recall well. But how would you do that? Those reaction vessels are quite big from what I´ve seen on the Internet/Dutch television. Do they apply cooling somehow?
Man´s main task in life is to give birth to himself.
Title: Heating or cooling a shaking reaction vessel
Post by: SPISSHAK on October 31, 2002, 01:36:00 AM
That's easy, for heat you would wrap electrical resistive wire (insulated nichrome) around it and hook it up to a variac transformer and calibrate solution temperature before commencing reaction.

For cooling I have no idea.
Title: cooling...
Post by: ClearLight on October 31, 2002, 01:51:00 AM
Wrap polyethylene tubing just like you did your wire around it and pump the coolant... or get a couple of those peltier electronic cooling devices and attach them to the apparatus..
Infinite Radiant Light - THKRA
Title: STP
Post by: terbium on October 31, 2002, 05:08:00 AM
The temperature should be kept around 50 °C when using Pt/H2 if I recall well.
Nah, room temperature and pressure work just fine and give yields in the 90-100% range. The rate at which the reaction sucks down the hydrogen will be determined by how vigorously one stirs.
Baseline Does Not Exist.
Title: Does just plain stirring work?
Post by: SPISSHAK on October 31, 2002, 05:19:00 AM
SWIM would like to set up something composed of a heavywall roundbottom filter flask, to a hydrogen in line, and a glass stopper greased and securly fit on the top by means of wire (kind of like a champagne bottle), put a spinbar in, set on a mag/hotplate, clamp, and go, if plain stirring would work this would be great!
Barring the filter flask you could substitute with a roundbottom (heavywalled) and fit a vacum adapter on top seal a glass stopper in the female end and setup up like that for hydrogenation.
I always thought for good H2 uptake you need agitation.
Title: Shaking is faster.
Post by: terbium on October 31, 2002, 05:53:00 AM
I always thought for good H2 uptake you need agitation.
Yes, the better the agitation the faster the hydrogen is taken up but vigorous stirring will work, shaking will be even faster.

Baseline Does Not Exist.
Title: The hollow shaft-stirrer is the best possible ...
Post by: Barium on October 31, 2002, 11:25:00 AM
The hollow shaft-stirrer is the best possible item to get the solvent saturated with hydrogen. A 2L reactor with cooling/heating coils and a hollow shaft-stirrer is the reference reactor all industrial sized reactors are compared to when designed. It is also the closest we have to an 'ideal reactor'.

A 1 foot long 1/4" stainless steel tube is bent to a spiral with a diameter of about 1.5" and the outlet and inlet attached to the reactor lid of a 1L reactor. This cooling coil is more than enough to keep any reductive alkylation or oxime reduction well under control. The reactor can now be placed in a water bath to heat it up to the desired temperature and cooling water can be passed through the coil.
Catalytic hydrogenation freak
Title: With pressures they put something it the rx ...
Post by: raffike on October 31, 2002, 06:56:00 PM
With pressures they put something it the rx vessel and shake the vessel with shaker that is driven by few hundred watter electric motor.It's pain in the ass to attach such overhead stirrer to rx vessel when pressures are involved.Raf's not fan of hydrogenating at the moment(he's messing with high scale metal dissolving reductions) but in future he sure will do some catalytic hydrogenations.Low pressure=fun,isn't it  ;)
A friend with speed is a friend indeed
Title: I think PtO2
Post by: flipper on October 31, 2002, 08:35:00 PM

NaBH4 route gives exellent yields.Only problem is that NaBH4 is expensive and might not be available for certain bees.Yields w/w go over 100%.
Then there's that platinum dioxide(Adams catalyst) method @ 3 atm H pressure with yields w/w in 90's.
Both methods are pretty cold.NaBH4 rxn contents must be kept under 10C,but i can't remember the temp needed in PtO2 method



The labs in holland use PtO2. I read in the a magazine overthere. Some chemists produced in order of some maffia people, in a week 300 kilo's of MDMA freebase. The gazzing and stuff was done in some other place. The people investigating the dismantelt lab couldn't trace the source of the PtO2.  8)
I think PtO2 route is cheaper if you re-use your catalyst a few times. Besides that you only need some Methanol, MethylAmine and MDP2P ofcouse.
NaBH4 route is so slow. To many hours work for 1 batch. Not practical. Only if SWIM make it for himself.  

Title: The kicker is
Post by: SPISSHAK on October 31, 2002, 10:01:00 PM
I think those Dutch are in such a favorable position because they get their ketone premade.
Is this true, they can just order the precursor custom made?
That would explain thier production capacity.
Title: So how do they get 300 kg per week?
Post by: lab_bitch on October 31, 2002, 10:21:00 PM
I once heard about this guy that welded together a continuous feed hydrogenator.  It was simply a large column packed with large diameter catalyst packing.  There was an outlet fitted with an expansion valve and an inlet connected to a positive displacement pump for the liquid reactants.  Once in the column, the liquid was continuously circulated down the column by means of another pump that pumped the liquid from the bottom of the column to the top.  The open space between the catalyst packing was filled with H2 that was supplied by a regulator connected to a tank of compressed hydrogen.  It could operate at fucking insane pressures like 200 bar!  The best thing was, he built it out of simple materials like stainless steel pipe and fittings.
Title: So how the hell do you vac distill 300kg of base ...
Post by: El_Zorro on November 01, 2002, 12:47:00 AM
So how the hell do you vac distill 300kg of base in less than a week?
Who is that masked man?
Title: Build a continuous distillation column.
Post by: lab_bitch on November 01, 2002, 01:43:00 AM
Build a continuous distillation column.
Title: OMG!! I think I just creamed my pants....... :-o
Post by: El_Zorro on November 01, 2002, 02:02:00 AM
OMG!!






I think I just creamed my pants....... :-[
Who is that masked man?
Title: HEHEHE!
Post by: SPISSHAK on November 01, 2002, 05:17:00 AM
Once again Madmax is true to form, how are things MRMax?
Have'nt heard from you in a while.
Title: Buy it in the Far East
Post by: Jackhammer on November 01, 2002, 08:17:00 PM
The Dutch have a natural feeling for trading. They obtain the MDP2P from countries like China. The estimate is that only 10% of all shipped MDP2P is found by the customs. Once in a while it is reported that they found several 1000 litres of the precursor. Hardly to believe what the Dutch production is....
Man´s main task in life is to give birth to himself.
Title: Very insightful
Post by: SPISSHAK on November 01, 2002, 09:21:00 PM
That's interesting.
I'd like to know more!
Title: Pays-Bas
Post by: GC_MS on November 02, 2002, 04:12:00 PM
In the Low Countries, large-scale production units don't always have to take care of their precursor materials, only for (more or less) OTC products. Organized crime delivers you the precursor material and pays the chemist to cook them some MD(M)A. It's because of the involvement of organized crime and profit-only attitude that I totally dislike this way of working. But whatever, it's the way things are over there.
Consequently, watching products as sassafras oil doesn't work that well (over there)... A couple of years ago, a Dutch farmer was busted. They traced him since he ordered massive amounts of sulfuric acid. He raised pigs, ordering sulfuric acid is very common for pig farmers, but not for the amounts he ordered. The Dutch police checked out his farm, and what did they find? Nothing! Exactly, absolutely nothing. However, the Dutch police watched him during his daily activities. Nothing special. But it was very odd that he drove his tractor in the middle of the night into the fields. They checked out what he was doing there, and yes... the pig farmer had a large-scale underground (!) XTC lab. This story was in the newspapers many years ago. Still, it is one of these stories one nevers forget  :) .
Ave Hive, synthetisandi te salutant!
Title: Busting labs
Post by: Jackhammer on November 03, 2002, 02:29:00 AM
I think once in two or three weeks a major lab is found in tha Lowlands. Most of the are pretty large. The funny thing is that in the papers you read they found thousands of liters of precursors. Actualy what is found in these occasions is just solvents. Sometimes they also find P2P, which, according to the newspaper, is a precursor for XTC.

Some pictures of these labs:

http://www.bka.de/pressemitteilungen/2001/labor/k_kevelaer2.jpg (http://www.bka.de/pressemitteilungen/2001/labor/k_kevelaer2.jpg)


http://www.bka.de/pressemitteilungen/2001/labor/kevelaer_gas.jpg (http://www.bka.de/pressemitteilungen/2001/labor/kevelaer_gas.jpg)


http://www.bka.de/pressemitteilungen/2001/labor/lab001.jpg (http://www.bka.de/pressemitteilungen/2001/labor/lab001.jpg)


http://www.bka.de/pressemitteilungen/2001/labor/lab002.jpg (http://www.bka.de/pressemitteilungen/2001/labor/lab002.jpg)


http://www.bka.de/pressemitteilungen/2001/labor/lab003.jpg (http://www.bka.de/pressemitteilungen/2001/labor/lab003.jpg)


http://www.bka.de/pressemitteilungen/2001/labor/lab004.jpg (http://www.bka.de/pressemitteilungen/2001/labor/lab004.jpg)


http://www.bka.de/pressemitteilungen/2001/labor/lab005.jpg (http://www.bka.de/pressemitteilungen/2001/labor/lab005.jpg)


Man´s main task in life is to give birth to himself.
Title: Hey wow! that's alot of hydrogen!!
Post by: SirSpicious on November 03, 2002, 03:25:00 PM
Just looking at those photos... what's the thing slightly left of center on the hydrogenator.. (the thing on the right) i can identify a manometer,thermometer, an engine (for stirring probably) in the center, but i can't figure out what that large thing is slightly left of center....
(no.. swiss isn't thinking of building a hydrogenator... just curious... i'm dreaming of building a still out of copper pipe at the moment =)
btw - do you think this deserves an award for 'tidiest' busted clandestine lab... all the rest i've seen photos are _really_ messy.. :-)
-SS

Even if you choose not to decide, you still have made a choice!
Edit: changed 'left' to 'right'...
Title: Very clean and professional
Post by: Jackhammer on November 03, 2002, 03:48:00 PM
You´re right. When looking at the pictures again, it is indeed very clean in this lab. Look at all the pipes and connections, I think they did quite a nice job in building this lab. I wonder what the capacity has been.... I´m not sure which photo you´re reffering to so I cannot say what it is you want to know
Man´s main task in life is to give birth to himself.
Title: The mysterious device....
Post by: SirSpicious on November 03, 2002, 04:34:00 PM
is best seen in pic in lab002.jpg.. the closeup in lab003.jpg cuts off part of it off at the top... it has some sort of guage on the the top.. it has a red tube that loops from (to??) behind the apparatus leading(see pic lab004.jpg) to a 'T' connecting to the vessel (nicely welded in stainless steel) perhaps it leads to the ducted air conditioning vents from the ceiling (air condensers???)

Even if you choose not to decide, you still have made a choice!
Title: It is an electric motor, looks about 1 ...
Post by: placebo on November 03, 2002, 08:50:00 PM
It is an electric motor, looks about 1 horsepower, connected with a shaft thru the stainless tube (probably with bearings) to the hydrogenator.
Intelligence is not the recall of knowledge, but the ability to use it. (Rainman was a retard)
Title: Looks like....
Post by: Jackhammer on November 03, 2002, 10:23:00 PM
a sort of funnel to me through which you can add solvents. There is a valve at the bottom, just before entering the reaction vessel so it is definately not a stirring device. Or does it measure the pressure? The picture is not very clear...

BTW is it normal to have so many (valve) connections on one reaction vessel? Methyl amine and hydrogen OK, but what are the others for?
Man´s main task in life is to give birth to himself.
Title: probably for purging
Post by: goiterjoe on November 04, 2002, 08:18:00 AM
They probably also have a nitrogen or argon inlet so they can flush the system prior to hydrogenating.
If at first you don't succeed, try, try again. Then give up. There's no use being a fool about it.
Title: Addition Funnel?
Post by: SirSpicious on November 04, 2002, 02:53:00 PM
It certainly looks like an addition funnel... perhaps they weren't running batches, and built a 'feeder' system... that could explain the large amount of cooling needed... hmm... there's another possibility..... i think it's a small hand pump! so they can take a sample their product to see if it's done yet...
-SS
Even if you choose not to decide, you still have made a choice!