here's a quick writeup to follow... these numbers are what SWIM follows, and are scalable. make a spreadsheet to save your brain.
17.8g MDP-2-P (100mmol)
20.3g MeAm (300mmol, 3x excess) mixed in 20.3g dH2O, then chilled
12.0g NaOH (300mmol, 1x ratio to MeAm, 25% solution) mixed in 36g dH2O, then chilled
SLOWLY drip the cold NaOH solution into the MeAm solution, chill.
110.7g MeOH, mixed with ~50mg HgCl2
7.6g Al Foil (280mmol, 2.8x excess) HD Reynolds
put into a 500mL RBF with condensor in this order:
stir bar
Al foil
MeOH and HgCl2 solution, swirl occasionaly until amalgamation started, then add...
basifed MeAm solution
then drip in Ketone.
if stirring cannot be acheived, swirl every 5 minutes during addition, and every 10 minutes until stirring gets going.
let react for 210-240 minutes.
premake 125mL 30% NaOH solution (37.8g NaOH, 88.1g dH2O), and let cool.
premake 250mL 5% NaOH solution (12.5g NaOH, 237.5g dH2O), and let cool.
slowly basify reaction with 30% NaOH solution.
extract basified reaction with 1x 200mL toluene, 1x 50mL toluene, combine.
perform A/B wash, titrate, dry, recrystalize.