H
	              |    H   H   CH3
	              C2    \ /   /
	            //  \    C   N
		   //    \  / \ / \
	       O--C3      C1   C   H
	   H2C/   |       ||   |\
	      \   |       || H3C H
	       O--C4      C6
	           \\    / \
	            \\  /   H
                      C5
		      |
	              H
.
.
.                     C11H15NO2
.
.     3,4-METHYLENEDIOXY-N-METHAMPHETAMINE
.
.                      EXTASY 
.
.
.
	      O
	      v
    O	   CH2CCH3
   / \ //\ /
H2C   |  ||	     +  H2NCH3  -- Methanol ->
   \ / \\/
    O
.
.
	MDP-2-P    +	Methylamine gas in Methanol ->
.
.
.
.
	      NCH3
	      v
    O	   CH2CCH3	   __> Extract with Silicagel
   / \ //\ /		  /
H2C   |  ||	     +	H2O	--- NaBH4 --->
   \ / \\/
    O
.
.
	IMINE	+ adsorped Water   --- add boro --->
.
.
.
.
	      NHCH3
	      |
    O	   CH2CHCH3
   / \ //\ /
H2C   |  ||
   \ / \\/
    O
.
.
3,4-METHYLENEDIOXY-N-METHAMPHETAMINE

NOTE : We know now, july 2000 , that it's much better to follow the basic rules from the P2P to Methamphetamine synthesis also for the MDMA and MDA synthesis, in fact you MUST use silicagel (pre-dried at 300 C for 2 hrs) in all relevant steps, especially, when you make first the imine and later the amine conversion by adding NaBH4 to the Imine.
MDP2P/Methanol/Methylamine mixing converts already to the Imine plus water, so you add silicagel to obtain the perfect results, for both MDA and MDMA and also for Methamphetamine.
So keep this in mind when you read the following texts.

The imine is formed when you mix MDP2P with 10% w/w MeNH2 / MeOH,( so then allready you must have added the 20% w/w pre-dried silicagel beads, to directly take up the water formed by the imine reaction mechanism), not when you crystalize, mixing acetone, that you do with the pure distillated freebase. No imine left there. The imine is hydrolized with the flooding with 8x water (ev. mixed with 5% NaOH or KOH, as Sunlight happily found out for the MDA One Pot ammoniumacetate and NH3 gas route ).
You see a picture of the total mechanism into the MDA route, with molecular drawing of the imine, right above here, many seem not to know what the exact mechanism is, it will help you out.

If you make the acetone/HCl mix in advance for the crystalisation of your destillated clean amine-base, you must use it as soon as you can, or it will even become red, depending on how much HCl you bubble in.
And add the acetone/HCl mix then slowly to the MDA (or MDMA or MDEA or Meth)-freebase while medium stirring, not the other way round, that would lead to decomposition when you start adding a part of your base, due to too acidic conditions.
It has been seen that vigorous stirring results in very fine crystals ; medium and at the end slow stirring results in more voluminous crystals, which is a logical effect of giving the crystals time and a more undisturbed medium to grow together.
The best is to keep your percentage of HCl fairly low, to avoid early decomposition.

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MDP2P--> MDA :

Materials : Still looking for the best yield possible, using basicly the description of the Methamphetamine ICE OnePot synthese (see below) and some minor or major changes, so you change only P2P to MDP2P and Methylamine to Ammoniumacetate or NH3 gas, see the ongoing discussions in the Methods forum for all possible improvements.
Changing the solvent, Methanol, to Glycol,  and Ammoniumacetate to Hydroxylamine f.e. could do the trick, research is going on.

Chemicals : The indicated route to MDA with Ammoniumacetate below will result in no more then between 30 and 60% yield for less experienced members, so for the time being you have to live with that, or improve yields by following the basic rules from the Methamphetamine One Pot.
Work with ANHYDROUS Ammoniumacetate, and dry all steps with Silicagel or MgSO4 or Na2SO4.
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Method :

To simplify life for you all, here's the ULTIMATE FOOLPROOF EASIEST WAY to make:
MDMA, MDA, MDEA (use ethylamine instead of methylamine) if you have the chems available!
A practical way to make Honey (tinted bases) is as follows:

  Parts	|  M D A -base		||	Parts	|    M D M A -base

   0,5	|  MDP2P (oil)		||	 1,0	|    MDP2P
   3,0	|  MeOH (solvent)		||	 3,0	|    MeOH
   1,0	|  A.Acetate (salt)	||	 0,3	|    MeNH2(gas)
   0,1	|  NaBH4(reductor)		||	 0,1	|    NaBH4

These quantity-parts are in weight!
So: you can choose if you want to work in gram OR kg.

Following starting quantity is 25 kg MDP2P or ev. gram, but then you must divide all other quantities by 1000, so kg's and/or liters ):

Prepare 6x20 L yerrycans in wich you can fill each 12,5 L cooled, (-20 C) MeOH. In each yerrycan you dissolve 1,25 kg methylamine in the cooled MeOH (methanol).Let the MethylAmine dissolve in the -20 C cooled MeOH which you already put in the freezer one night before!
Use a upside down laying gastank with MA (30-45' angle)and fill with a thick synthetic black rubber hose the liquid-MA as deep as possible in the MeOH. SLOWLY! It takes ca. 10 min., per yerrycan.
The yerrycan stands on a digital balance, so you know the weight added.
Surround the hose with a wet towel at the filling opening of the yerrycan for the unhealthy smell.
When ready fill all the yerrycans with the MeOH/MeNH2 mix in the reactiontank. [Add in case of (MDA) now the AAcetate (in the pure methanol) instead of the MeNH2 gas !].
Cool now the reactiontank to +5 C and start the mixer anticlockwise, so the fluid circulates from bottom to top. This way no air is mixed in, so less oxidation. Add at +5 C the 25 L. MDP2P .(pre-cooled).
Start then directly (because a slow reaction starts already), every ca. 5 min, addition of the NaBH4, ca. 3 soupspoons per time. Use a funnel and wash every time with a little methanol. Keep all holes closed inbetween or it stinks! Because of the excessive cooling the temp. will not rise much, only to +15 C. Wait again till ca. +7 C to add again. Are you impatient and add to quick, then the mix will start heating, evenso boiling! This may never occur,then your product will be lost !
This process takes ca. 7 hours. Ending temp. will be ca. 25 C. Stop after 7 hrs. the cooling and let react with mixer on for 29 hours.
After this time, you prepare 200 L clean water, which you mix with 10 Kg NaOH or KOH, until all is dissolved.
This 5% water/NaOH-mix you add to the cooling tank (fast), then you measure the pH, should be between 11,5 and 12. (If you add coincidently acid instead of NaOH base, greenish fat form in and on the fluid). Stop after 10 min. the mixer and let the raw brown base precipitate 30 min to the bottom and tap off the base through the valve at the bottom. Stop tapping when you see lighter color (water) coming.
Add now 3 liter methylenechloride (dichloromethane=CH2Cl2) to the tank, mix 10 min., stop the mixer, wait again 30 min. and tap off the rest of the base, now diluted in the CH2Cl2.This gives totally ca. 43 L raw base.
Now we remove the CH2Cl2, Methanol and the water in a simple distillation setup, with low vacuum circa 500 mbar, with magnetic mixer/heater, mixerpin teflon, glassware with NS29 connections ( 20 L 2-neck flatbottom flask PYREX!, thermometer, cooler 60 cm, glas-alonge and 10 L collecting flat-bottom erlenmeyer flask).
Start at 35->55 C for CH2Cl2, then 55->85 C for methanol and 130 C for all the water. Re-use the CH2Cl2 and the methanol! Now you are left with ca 28 L half-clean MDA or MDMA amine-base (depending on the fact if you used Am.acetate or MeNH2 gas, colour is light brown).Now we will clean the raw base by 2 times recrystallisation with acetone 98%, (m)ethanol 98%, and after that washing min. 3 times with acetone 98%. Use 20 L P.P. plastic buckets to do this.
Mix 5 L base (cold) and 10 L icecold acetone. Leaf inductionmotor-mixer on. Bubble HCl-gas 99% through with 1 meter StainlessSteel pipe, (inner diameter min 5-8 mm) until white crystals form. Stop when pH= 7,0 and start with the next 5 L base. The first one will rise again to ca. pH=8,0.
Later you can bubble again a littlebit HCl-gas through until again pH=7.0 or even to pH 5.0 . Let the crystals precipitate and pour the upper acetone off.
Re-dissolve the wet crystals now in the minimum quantity of HOT(nearly boiling) methanol or ethanol in a metal bucket (because its hot !) until you see no more crystals, so you now have a saturated solution in (m)ethanol!
Pour 5 L of this solution back in the plastic bucket, and add 5 L Acetone, which is -15 C.
When cooling down, you will see crystals form again,in a dirty solution. Wait until no more crystals come, pour off again and dissolve again in hot (m)ethanol. Do this as many times until you have snowwhite crystals. Dry on glasplates on the floor with blower.
You now have H(M)ONEY in the Bank.

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MDP2P--> MDMA Another write-up.

Materials : idem

Chemicals : idem

-------------------------------------------------------------------

Method :

-------------------------------------------------------------------
Preparation of MDMA by reductive amination with sodium borohydride
by Labtop (written by Quicksilver, editted by LaBTop)
-------------------------------------------------------------------

- Introduction

Until recently reductive amination with NaBH4, for the production of MDMA, was assumed to be inferior to the well-known NaCNBH4 route (that has been popularized by Alexander Shulgin for the production of MDA) and other synthetic routes, like aluminum amalgam. The following method proves that the NaBH4 reduction actually is superior to all other common routes used in clandestine chemistry.
The method is relatively simple, it doesn't require complicated equipment. The work-up on the reaction mixture is simple and efficient. The method is very usefull for big scale production of MDMA and gives high yields (+90%!).
There is a relatively rapid formation of the imine and the imine is reduced relatively rapidly.
There's no reduction of the ketone to the secundary alcohol, as one might expect(2). In similar reactions, the water!! that is produced during the forming of the imine (Schiff Base) is removed from the reaction before the imine is reduced.
As we know now,much better with pre-dried (3 hrs in oven, 300 Celsius) Silicagel beads, 3-5 mm diameter, take a quantity of 20% weight compared to your MDP2P weight. Because of the stability of the imine, this is not necessary for the production of MDMA, but should in fact allways been done, to reach maximum yields !
This reaction is an improvement of a known synthesis (1), a similar reduction in an aqueous sollution of ethanol was performed, but the yields were only 31%.

- Synthesis :

MDP-2-P + methylamine-> intermediate imine +H2O-> MDMA freebase-> MDMA HCl salt.

- Ingredients
MDP-2-P 1000 g
Methanol 3000 g (>99%)
MeNH2 (gas) 300 g (99,9%)
(Be very carefull with MeNH2-gas: it is toxic and carcinogen, but when handled with care, no problems.
I advice to not use a gasmask, because when you smell it, you can avoid it, but with mask you are not warned and it can be uptaken through your skin! Use wet towels to avoid problems at ev. leaking points!).
NaBH4 100 g .
(NaBH4 is a common reducing agent. Do not spill NaBH4 on hands or face without noticing it(e.g. whiping sweat off your face), or you will be punished with red spots there which will never go away!
It takes minutes before you feel the pain, and then its too late.
So wash face and hands with water, frequently.).
filtered clean H2O.
33% HCl .
conc.NaOH solution .
DCM (DiChloroMethane).
Acetone >98%.

- Equipment :

*-- There are several options for the reaction vessel. One could think of a 500 to 1500 L stainless steel milk cooling tank, that is modified to ones needs. But a fermentation tank (plastic or stainlees steel, from 20 to 8000L), with small modifications will do just as fine. Or one could buy a 1m3 (=1000 L.) plastic tank everywhere at second hand tank and cans stores. Have a handy manhole to clean, are totally airtight and as a bonus, have a nice tap-valve at the bottom.They ship NaOH ,33% HCl etc. all over the world with them.
*-- A solid diaphragm vac.pump is recommended for the vac. distillation. For example a Vacuubrand Type MD 4C, 3.0 m3/h. It sucks from 1.7 to 11.2 m3/hour, ask for Chemistry Design(PTFE) series.
*-- MeNH2-gas is made by reacting MeNH2.HCl with conc.NaOH. (An other option is to react 40% MeNH2 with dry KOH.) (I will add a lot more on MeNH2 synthesis shortly.)

- Step by step :

1) Preparation :

Dissolve 300 gram, not ml ! methylaminegas in chilled 3000 gram methanol (-20 C). Cool in the mean time the reaction-mixture to +5 Celsius.
Start the mixer (anticlockwise so no air is mixed in) and add the 1000 gram MDP-2-P.
NOTES: Make 300 gram MeNH2-gas by reacting MeNH2.HCl with NaOH. Or dissolve the methylaminegas at hand from a gas cylinder in methanol, using an upside down laying (45 degree's) gascylinder with (fluid) methylaminegas in it, no pressure regulator on it. Attach a thick black synthetic rubber hose to the valve, open that valve slowly ,while the hose is down at the bottom of your first jerrycan with icecold Methanol, which stands on a big flat digital balance. Surround the hose with a wet towel. Add slowly 300 gram gas in the jerrycan. Be aware of a popping sound when the gas implodes when it enters the Methanol. Don't let suck back, close the valve everytime suddenly.

2) Reaction :

Start adding NaBH4, one teaspoon ca. every 5 minutes, H2-gas bubbling has to disappear before adding again, temp. should be between 8-18 deg C. (Wash down with methanol). Adding of the white NaBH4 powder will take 7 hours. With mixer on let it sit for 29 hours more.(4 hours will do for people that are in a hurry,loss 20-30% yield).
NOTES: When the reaction vessel is opened it should be covered by a wet towel, so the methylamine-gas can be absorped by the water. (1 L water absorps 1000 L NH3.) An airlock might be sufficient for that goal too.
Do not airtight the flask, let a thin tubing out the window,wrapped at the end with a WET towel!

3) Work-up I :

Leave the mixer on. Add 8 L clean H2O with 1%=80 mL 33% HCl. (The 80 mL HCL is redundant, don't add it at all!).
(When making MDA as your endproduct, you add 5 weight % NaOH or KOH to the water, to facilitate a good separation in the following separation procedure).
Liquid will be greenish brown, pH=10,5 (11,5 is better than 10). !!When green soap possibly starts to form: you made a mistake, you added far too much HCl ( To avoid any risk: do not add it at all. Redundant!!)...
Brown freebase will sink to the bottom of the vessel. Tap off, till a bit clear water is coming out of the valve. Close then the valve. Add 200 mL DCM to the reactionvessel and mix for 10 min. Stop the mixer and wait 30 minutes. The DCM with the rest of the freebase will sink to the bottom. Tap off. Combine the two. There will be app. 1750 mL of base fluid + DCM.

NOTES:

You can again basify the water with conc NaOH sol. to pH =13-14 and tap off the last oil.
The 8 mL 33% HCL (1%) is added to the water to make sure any unreacted NaBH4 is neutralised, but is not needed, in the following steps this is taken care of automatically.

4) Work-up II :

A vac.distillation setup is prepared. First the methanol, DCM, water and other lowboiling stuff are removed, then at 165 C the clean freebase comes over. Approx. 1.0 L. freebase.

NOTES:
Step 1. The water and other lowboiling stuff comes over at 130 C. Remove when nothing more comes!
Step 2. Set on 165 C. At first around 140-145 C you see the first little drops of clear oil condensate and at 160-165 C and 20-18 mbar it starts Running!
To distill of the water, methanol and other low boiling stuff from the reaction mixture, the use of an aspirator is sufficient! To get the freebase out, the use of a decent vacuum pump is recommended.

5) Crystallization :

Mix the base 1:4 with clean,cold(-10 to -20 C) acetone and bubble through with a Stainless steel pipe 8 mm x 1 meter with HCl-gas 99%. SLOWLY! After ca. 5 min a thick, white crystal mass will form. Check frequently with pH-meter ( aquarium shops sell good ones from Hanna Instruments for circa US$ 60.- ), or pH papers from Merck, until pH = 7 to 5 . If the mix get too hot, place back in big freezer to cool and proceed with next cold batch. Be very carefull not to go under pH=7 to 5, because then your powder will solute again and you must add base again until pH comes up again to 7. So keep always at least 20 mL freebase ready in case of mistakes ! Dry the acetone/powder mix in a Buechner-funnel with aspirator vacuum. Dry again on glassplates on the floor under airconditioner or slow blowing fan's in a dry room.

- Epilogue :

There are reasons to believe that the salt form of the amine can be used, ( I don't think it will be interesting, without high decrease of yields LT/ 10-07-2000) but the gas method is by far preferrible.
Ethylamine can be used to produce MDEA.
Ethylamine is a gas above 17 C, but a fluid under 17 Celsius, so very convenient when first placed in a freezer,  just pour it in the icecold methanol then.
Ammonium acetate or NH3 gas to produce MDA is another possibility, Sunlight and Cesium have researched the Ammonium Acetate process further and reached yields of ~ 50-65 %.
The same method was tried with P-2-P, first with unsatisfactory results when NO !! water was removed, because the imine that's formed here isn't as stable as the MDMA or MDA imine. When you remove the water while forming,with a drying agent, Silicagel, this also works (12-07-2000) perfectly, even better !!! Quantitatif yield near 100%.
 
- References

1. Noggle, F. T.. Jr., DeRuiter, J., and Long, M. J.. "Spectrophotometric and Liquid Chromatographic identification of 3,4-Methylenedioxyphenylisopropyl-amine and its N-Methyl and N-Ethyl Homologs." Journal of the Association of Official Analytical Chemists, Vol. 69. No. 4. 1986, pp. 681-686.
2. Shellenberg. K. A.. "The Synthesis of Secondary and Tertiary Amines by Borohydride Reduction." Journal of Organic Chemistry, Vol. 28, Nov. 1963 pp. 3259-3261.
3. J. Weichet, J. Hodorova and L. Blaha, "Reductive amination of phenylacetyl-carbinols by sodium borohydride." Coll. Czech. Chem. Commun. 26, 2040-2044 - CA 56, 5864c (1962)

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

MDP2P--> MDEA :

Materials : Same as for MDMA.

Chemicals : Same as for MDMA, except :

1.--- A equimolar amount of Kg Ethylamine, CH3CH2NH2, compared to the amount of Methylamine in above One Pot's. A gas at +17 C, a fluid gas under that temperature !

-------------------------------------------------------------------
Method : Same as for MDMA.
Only switch methylamine gas for ethylamine gas or fluid-gas.


~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~
~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~