I wonder if it's all right with the process .. please

5g - PdCl2
350g - p-benzoquinina
1200ml methanol
150ml water

mix everything in a big balloon

was added slowly to

600g - safrole
200ml - methanol
mixed

added every 12 minutes ...

.................................................. ................................

reduction for I did ..

250g - mdp2p
1500ml - methanol
500g - ammonium acetate
25g - NaBH4 (addition over 4 hours, always at low temperature of 8C)

.................................................. ..............................


throughout the order process is correct?

could be made to mdma, substituting ammonium acetate for methylamina HCl (powder)?

in the synthesis of labtop, methylamine gas is used .. (Could be replaced by methylamine HCl (powder)?

which the income you would expect from all this?


thank you

To turn your MeNH2 into a gas it will need to be made basic. To do this take a flask which contains a molar excess of NaOH as an 50% aqueous solution. Add your MeNH2.HCl. Stopper the flask with a hose coming out. That hose will lead into trap to prevent the MeOH from being sucked back into your rxn vessel. (If you want everything dry it will then lead into another flask filled with a dessicant b/w the MeNH2 flask and the suck back flask) then from this your hose will attach to either a pipette or a gas dispersion tube, that will be in a flask of stirred MeOH.

Heat the flask slowly (not above 80°C or you will get water coming over too) with the MeNH2/NaOH   with stirring to drive off your MeNH2 and bubble it in to your flask of MeOH. You want the MeOH to be as cold as possible. Weigh your flask of MeOH periodically to see how much MeNH2 has been absorbed.

et voila!

You might want to do this out of doors, in a garage or in a fume hood or its going to smell to high heaven like dead fish.

Why you choose this route starting from safrole?  Jon's method Bromo/Iodo Safrole looks like more easy and effective (all Right may be effective as the same, but more funny and cheap no doubt)
I think this route is fine if you start from piperonal=> MDP2NP> MDP2P=>MDMA. But from safrole Jon is the best.

I know RoidRage, lot of information for bromo and iodo, but when methylamine going to IPA, the workup is something like a mystery.
Anyways i think than Jon has written enough to give it several tries until it works. Maybe drying agents is the key for the real success.
Amination at room temperature sounds like a dream.
And the best is than Jon is here, with one PM one would be lucky enough to find the way. 

check this out mdhard

really appreciate your great help my friend ...

I'll read the article with a lot of attention.

thank you very much

alkylamine.hcl + lots of solid naoh (6g per g of water present/formed in the neutralization), slurried and stirred in toluene (sitting in an icebath) for 30-60 minutes. then the mixture is left to settle for some minutes more and the toluene is decanted from the solids and quickly filtered to give a clear, dry alkylamine/toluene solution suitable for imine formation.

Often the imine formation reaction is done with alcohol as solvent. If so, the solid base must be removed very efficiently or the rxn will fail.

Diethyl ether maybe a better choice than toluene.

For the reaction using MeAm, don't use MeAm.HCl. Better to gas methylamine in methanol, if you know how to do it well.

I tried it once and failed, I wasted 30 g of MeAm.HCl.

The technique I like most is, add MeAm.HCl to methanol ( better cool it first ) inside a bottle. It will sink to the bottom. Next, add the same molar amount of NaOH. It will also sink to the top of the MeAm.HCl layer. Stopper the bottle WELL.

Let it react a bit, then turn/shake the bottle, finally shake it hard. It will become all white like a milkshake.

Let it stay inside your refrigerator for a few hours ( better make it one day before using ).

Then, decant the top clear ( light yellow color ) liquid, discard the bottom white solids.

Place the liquid inside your boiling flask, add the ketone, turn on your stirring, cool it in ice and water and proceed.

You can achieve 65 % yield.

For small amounts of MeAm.HCl, it is a better technique, more control over the amount you are using and no waste from gassing it in methanol.
 

65% is the consistent number i see appear when this is done under hydrated conditions.
consistently..
i liken it to the golden ratio, and the fibonacci sequence, established immovable numbers.

@xman47, the the hydroxide in the methanol is reacting with your ketone thus accounting for low yields. You should use a different solvent for the amine neutralization.