Before SWIM tries to make some honey, he wants to make sure that he has a good procedure to follow. He thinks, "I'll post it to the Hive and the nice bees there will point out the bad parts and hopefully add some good ones". Feel free to post any comments/suggestions.
SWIM plans on using an oil bath through this procedure. Just thought I should mention that.
Synthesis of MDMARXN: Wacker Oxidation of Safrole -> MDP-2-PIn a 2L flask, add 400mL MeOH and 2g PdCl2 and stir for 2½ hours
Add 120g p-Benzoquinone and 50mL dH2O and continue to stir for 1 more hour
Mix 160g Safrole and 50mL MeOH in an addition funnel and add over 1 hour with continuous magnetic stirring
Solution should turn a very dark red-orange
When the reaction is finished, heat to 70°C for 3 hours
Flood rxn mix with slightly acidic water and mix contents thoroughly
Decant organic layer and save
Wash aqueous layer with 2x100mL DCM and save
Combine organic layer and DCM washes
Wash with 2x200mL each 10% NaOH, saturated NaCO3, and saturated NaCl
Dry with 50g anhydrous MgSO4
Combine organic layers in a 500mL RBF
Vacuum distill the MDP-2-P
To further purify, vacuum filter through activated charcoal a few times
Theoretical yield
RXN: Al/Hg/MeNH2 Amalgam of MDP-2-P -> MDMAOn a 2L RBF, place a Claisen(?) adapter fitted with an addition funnel and a condenser
Add 400mg HgCl2 dissolved in 750mL to the flask and turn on the condenser
Turn up heat to boiling, then let cool and add 33g prepared (according to the Dr. Gonzo photoessay) Al foil
Start magnetic stirrer
Mix 31g MDP-2-P, 25g MeNH2, and 50mL MeOH in an addition funnel
Open valve on addition funnel to about 3 drops a second, or enough to maintain a steady reflux
When the rxn starts to slow down, add another 75mL of MeOH and let sit for 1 hour
Mix 700mL dH2O and 262g NaOH in a beaker
Dump the rxn contents into a 4L beaker (add MeOH to loosen sludge)
Add the NaOH solution to the beaker
Stir the mixture for about an hour
Add 500mL Toluene and stir for a few minutes, then layer
Wash the sludge with 2x250mL Toluene and save
Combine Toluene layers
Wash 2x with saturated NaCO3, once with saturated NaCl, and once with dH2O
Drain into a clean beaker with 35g anhydrous MgSO4, stir, and let sit for ½ hour
Filter into a very clean beaker and wash the MgSO4 with a little more Toluene
Gas with anhydrous HCl until MDMA precipitates out of solution
When solution becomes cloudy, cover the beaker and place in the freezer for ½ hour
Vacuum filter the precipitate and repeat process until no more MDMA is produced
Dry crystals
Theoretical yield
Synthesis of Precursors:HgCl2 synthesisMeasure 20g Hg and place in a 100mL conical flask with an exhaust tube
Add 60mL conc. H2SO4 to the flask
Bubbles of SO2 will rise from the H2SO4/Hg interface
Maintain a vigorous bubbling of SO2 by adjusting the heat
A white crystalline deposit of HgSO4 will appear
The Hg should be completely reacted after about 30 minutes
Allow the reaction mixture to cool and pour off the acid
Pour the crystals into 750mL hot dH2O and filter
Slowly add this solution to 500mL saturated NaCO2 until red-brown precipitate forms
Filter off the precipitate
Repeat until there is no more precipitate
Wash precipitate with dH2O
Place in a 500mL beaker and create a suspension with 20mL dH2O
Make up a solution of 20mL HCl in 100mL dH2O
Add this to the suspension in small quantities with good stirring
Stop HCl addition when the precipitate color changes to white
Neutralize solution
Cool, filter, and dry crystals
Recrystallize from boiling dH2O to purify
Theoretical Yield 19.37g HgCl2
(I'll be trying a scaled down version of this with 1.2g Hg that I recovered out of a broken thermometer since you only need <1g anyway)Benzoquinone SynthesisIn a 500mL Erlenmeyer flask, place 23g hydroquinone
Add 17.5mL 93% H2SO4 in 250mL dH2O with low heat until hydroquinone dissolves
Plunge flask into an icebath and stir vigorously to obtain a crystal suspension
Remove the flask and add 35g K2Cr2O7 in 60mL dH2O over 10 minutes while swirling
Keep reaction temp under 25°C
The green-black quinhydrone complex will precipitate, then change to yellow-green
Cool mixture to 5°C and filter Benzoquinone crystals
Wash with a small portion of ice cold dH2O
Theoretical yield 14g
I have a few questions:
Any ideas on the theoretical yeilds?
Is Benzoquinone the same as p-Benzoquinone? If not, how can I convert it?
I know that Xylene can be used in place of Toluene. Are there any other solvents that can be replaced?
Does anyone see any difficulties that may be involved in this? Any improvements that I missed?
trancendence through neurochemistry