Application: It is one of organic intermediate, like AMG-510
It can be get by one step reaction of S-2-Methylpiperazion
Detail of preparation:
Add water (500g, 5w/w%) into the reaction bottle. Add (s) -2-methylpiperazine (100g, 998.4mmol, 1 equivalent) into the reaction flask with stirring. Add HCl (36% aqueous solution, 102.1g, 1008mmol, 1.01 equivalent) and methanol (200g) into the reaction flask with stirring. Add the solution of boc2o (222g, 1008mmol, 1.01 equivalent) in methanol (200g) drop by drop into the reaction flask at 15-25 ℃, and then stir at 20-30 ℃ for 18 hours. Evaporate the contents of the flask to dryness under vacuum at 40-50 ℃ to form a residue. Water (500g) was added to the residue and the mixture was stirred for 1 hour. The mixture was filtered and the collected solids were washed with water (50g). Extract the aqueous filtrate with ethyl acetate (500ml). Adjust the extracted aqueous phase with 30%naoh to a pH of more than 12, and then extract it three times with ethyl acetate (500ml). The organic phase was washed twice with brine (500g) and then dried with anhydrous Na2SO4. The dried mixture was filtered and the collected solid was washed with ethyl acetate (100ml). The filtrate was concentrated to dryness in vacuum at 50-60 ℃ and further concentrated in high vacuum (5mm Hg) at 65-75 ℃ for 3 hours to obtain (s) -4-n-tert butoxycarbonyl-2-methylpiperazine. The purity was 97.7%, the content was 95.9%, and the yield was 76.4%.
Post time: Jun-27-2022