          >>> SYNTHESIS OF MMDA FROM PARSLEY LEAF OIL ENTIRELY OTC <<<

>STEP 1 - Purification and extraction of myristicin from parsley leaf oil<

Obviously, the best way to do this would be by fractional vacuum distillation.
But if you don't have this, wash w/ an equal volume of 5% NaOH, followed by 3x
w/ half the volume of dH2O. If you have a problem separating the layers,
saturate w/ a little NaCl. Now dry your myristicin by heating @105C until all
bubbling ceases.

>STEP 2 - Iodination of myristicin<

Okay. For this you will need to generate HI. You can do this either by dripping
dH2O onto RP/I2, or phosphoric acid onto I2. You need an equimolar amount of HI
to myristicin. FW of myristicin = 193.224. FW of HI = 127.912. So for every 10g
myristicin, you'll need 6.62g HI. Let's call it 7g. The equation for producing
hydrogen iodide from iodine and red phosphorus is

16H20 + 10I2 + 2P4 ---> 20HI + 4H3PO4 + P4,

so for every 7g HI you'll need 6.94g I2, 0.17g RP and 0.79mL dH2O. So get a 50mL
bottle, punch a hole in the lid and epoxy 2 tubes in place, one short one and
one long one. In the short one, put an addition funnel containing dH2O. Epoxy
the other end of the longer tube thru the cap and in to the bottom of a second
50mL bottle, filled w/CaCl2 to dry the HI. Another tube comes out of this
bottle, going into the top of a third 50mL bottle, which accomadates for
suckback. Out of this bottle comes another tube, out of which dry HI will come.
Make sure everything is sealed FIRMLY w/ lots of duct tape. Keep the container
with your myrsticin in in an ice/salt bath. Add 1mL dH2O, slowly and watch your
myristicin iodinate. Or scale up.

>STEP 3 - Purification of crude iodomyristicin<

Unless you can ditil it under vacuum, take your just-iodinated myristicin, and
wash w/: half the volume of 5% NaOH (2x), dH2O, then chill to 0C and wash w/
half the volume of cH2SO4, also chilled to 0C, then w/ 3x dH2O.

>STEP 4 - Preparation of concentrated NH3 in MeOH<

The idea here is to bubble NH3, made from NaOH and (NH4)2SO4 (ammonium sulphate
fertilizer), into anhydrous MeOH, as cold as possible. So, the rxn to make the
NH3 is: (NH4)2SO4 + 2NaOH -> 2NH3 + Na2SO4 + 2H2O. You want a 10x molar xcess of
NH3 to myristicin, so to be on the safe side slowly drip 40g aq. NaOH onto 67g
ammonium sulphate fertilizer. Use the same set up as for the HI generator, sept
dry w/ NaOH instead. Bubble thru 35mL anhydr. MeOH in an ice/salt bath.
Pre-chill the MeOH in a freezer to bout @-11C. This is for 10g myristicin.
Obviously u can scale up for more.

>STEP 5 - Amination<

Now get another bottle, and mix the iodomyristicin and NH3 in MeOH together,
screw the lid on *tight*, and wrap up with LOTS AND LOTS of duct tape. Store for
1 week and shake vigorously regularly. The higher the temp., the faster your rxn
will go, but make sure your container can withstand the pressure and also
unwanted side-rxns generally tend to occur more at higher temperatures.

IudexK <iudexk@dangerous-minds.com>

kudos to Strike, piglet, Shulgin, the hive.

- - - - -

I think it is important to point out that if iodination is not carried out 
slowly, or the distance from the end of the iodination tube is not sufficiently 
deep, it may be necessary to generate a large excess of HI. Completion of the 
rxn can be determined by weighing the supposedly iodinated myristicin to see if 
the weight has increased by the expected weight. Also, there appears to be a 
large variation in the constituents of parsley leaf oil, myristicin content
varying from 2% to 90%, so knowing the constituents could be helpful. Other
allylbenzenes present are predominantly apiole and TMAB. It also seems
there is a difference in some cases between parsley herb and leaf oils.


IudexK
