-------------------------------------------------------------------------------
            MDA by reductive amination with Sodium Cyanoborohydride
-------------------------------------------------------------------------------

Into a 5 L flask on a stirplate place the following:

a big ass stirbar (Turn on the stirrer!)
1.5L of anyhydrous methanol
920g of ammonium acetate

Note: add slowly and make sure that the acetate dissolves ok, the addition of
acetate and methanol is endothermic and the solubility of it will go down, if
you are not careful you will get a dome of acetate covering the bar and no
movement of the solution!!!

PUT ON GAS MASK HERE

Into a 1L beaker place the following:

146g of sodium cyanobrohydride
500ml anyhdrous methanol

Stir with a glass rod, teflon stirbar retriever or something similar to knock
out out all the chunks/goo of sodium cyano, note that it is fizzing and popping,
do not reccomend breathing the fumes . Now into that 1 L beaker of fizzing cyano
mix, add: 400g of MD-P2P. Stir it a little and quickly add it to the 5L flask.
Oxygen degrades cyanoborohydride very quickly so this shouldnt take more than a
minute or 2 from the time you open the container of cyano (pre weigh everything
else.) Now take a balloon and fill it HALFWAY with nitrogen. Toys 'R' Us sells
these punch balloons that fit nicely over a 24/40 joint. Anyhow take the N2
filled balloon and spray a little bit into the flask to get rid of the
atmosphere in there and then place the ballon over the neck of the flask. Let
stir 48-72 hours. Solution should be clear with a light tinge of whatever color
your ketone was. You can take your gas mask off now

Note: during the 2-3 day wait, make up about 2L of saturated NaOH (lye) solution
and freeze it.

After 48-72 hours, take the balloon off and distill off the methanol. It will be
the first fraction that comes over and you should get what ya put in (~2 L).
After the methanol is distilled off, cool the flask in an ice bath with
stirring. If you got all of the methanol out whats left will more than likely
polymerize (solidfy) into a big white mass. This is perfectly ok.

Once the contents of the flask have cooled (<40C), CAREFULLY add 2L of 10%
HCL(roughly 660ml muriatic and 1340ml distilled H2O.) Add slowly and make sure
fizzing doesnt get out of hand or you will be wearing it!!! Let stir for a few
minutes until all of the polymerization has broken up. Now dump half this into a
4 sep funnel and extract 2x200ml DCM. Then do the same for the other half. Save
the dcm and freeze it, it contains any unreacted ketone and can be reused,
simply boil off the dcm to know how much ketone ya got. Ketone can only be
recycled once, after that it degrades.

Now take the goods and put em back into that 5L flask in the ice bath
(stirring). Now CAREFULLY add that cold saturated NaOH solution you made until
you get to ~pH 11. It WILL fizz and you WILL paint your ceiling with this stuff
if you dont add slowly and carefully. Don't add all 2L that you made up, just
check the pH every now and then until it gets there. At about pH 9 you'll start
to see amber oil fall out...thems the goods and its a damn pretty sight to see.
Let it stir for a few minutes and then put what ya can in the sep funnel.
Extract 3x200ml DCM AT LEAST...too much dcm dont hurt here. It usually turns red
when ya do this too (anybody know why?) Anyhow that white cloudy water stuff
will get clearer and clearer the more product you extract. Take the dcm/freebase
oil and freeze till ya ready to xtallize. Dry thru a filter funnel of sodium
sulfate and gas. Very clean and very pretty snow. You should get at least 200g
of product.

This method scales nicely and I dont know people who run this rxn at 3 times
this scale in 12L flasks on a weekly basis. For you experienced bees, the 5x
molar excess of acetate vs. the 10x doesnt seem to effect yields. Also while not
having had the opportunity to test it, silica gel during that 2-3 wait has been
said to improve yields ~25%.

P.S. After adding the NaOH solution be sure that the entire contents of the
flask have cooled <40C, otherwise when you add the DCM it will BOIL!!!
