MDP2P to MDMA route

[dennispeck]

What do the Dutch mean when they say  : "the cold method"  ??

[SPISSHAK]

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.

[Jackhammer]

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.

[SPISSHAK]

I don't think anything will happen at zero centigrate.

[Jackhammer]

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  

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.

[SPISSHAK]

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.

[Jackhammer]

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.

[El_Zorro]

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?

[carboxyl]

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.

[Sunlight]

May be it is the NaBH4 procedure that LabTop gave us. The best yields and low temperature.

[raffike]

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

[Jackhammer]

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.

[SPISSHAK]

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.

[ClearLight]

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

[terbium]

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.

[SPISSHAK]

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.

[terbium]

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.

[Barium]

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

[raffike]

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

[flipper]

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.  
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.