It's been a while since last pictured writeup so raf thought he'd post one.This one is about reductive amination of MDP-2-P with activated aluminium and methylamine.
Al/Hg a la Os/BrightstarIngredients: 60 grams of very good quality PMK
30 grams of 0,1 mm Al foil
95 grams of methylamine.HCl(home-made)
450 ml of denatured(25% IPA,rest is EtOH) alcohol
40 grams of NaOH for methylamine liberation
0,5 grams of HgCl2(reagent grade Fluka)
50 grams of NaOH for post-rx dilution
0,5 liters of Xylene
Procedure:30 grams of aluminium foil(0,1 mm,cut to 2 x 2 cm pieces and slightly folded) and alcohol was added to 3 liter 3-neck RB:
Methylamine.HCl(homemade and little moist from chloroform,raf uses big excess,methylamine is very easily and cheaply made,see Rhodium archive or another picture-essay by raf) in 100 ml water was basified with 40 grams of NaOH in 120 mls of water:
Ketone was pulled out of freezer:
Ketone was dissolved in some 100 mls of ethanol:
Ketone solution was poured to addition funnel.Methylamine solution was poured to reactor along with mercuric chloride:
Overhead stirring was started.Soon aluminium was amalgamted and ketone addition started:
Temp constantly rose(1-2 degrees a minute) and in 30 minutes ketone addition was completed.Temp was kept around 60 C with external water cooling.About 1 hour from start,rx started to calm down and was left to stir another hour.No unreacted aluminium was seen.Whole slurry was poured thru funnel to 5 liter sep funnel and 2 liters of water along with 100 grams of NaOH was added.Solution was washed 3 times with total of 0,5 liters of Xylene and xylene was then washed 3 times with water.Freebase in xylene:
Gassing apparatus(sulfuric acid+hydrochloric acid-->HCl gas,sulfuric acid in addition funnel and hydrochloric in flask) was built from pressure equalized addition funnel and flask.Gassing tube is PTFE.Freebase is constantly stirred with magnetic stirring.
Freebase after gassing:
Product after purification:
Yield 42.8 grams(that cup weighs exactly 3 grams):