Piperazine, 3-methyl-1-(methylsulfonyl)-, (3R)- synthesis

Yield:1354947-83-3 20.02%

Reaction Conditions:

with sodium hydroxide in tetrahydrofuran at 0 - 20;

Steps:

A solution of methanesulfonyl chloride (6 g, 52.4 mmol) in THF (50 mL) was added, over 2 min, to a solution of (R)-2-methylpiperazine (5 g, 49.9 mmol) in NaOH (2M) (50 mL) and THF (50 mL) at 0°C. The reaction mixture was stirred at 0°C for 1 hour, then left to warm to room temperature overnight and poured onto 2M hydrochloric acid (100 mL). The mixture was washed with ethyl acetate (3 x 50 mL). The aqueous phase was separated and basified (pH=12) by the addition of solid sodium hydroxide. The mixture was extracted with DCM (2 x 100 mL). The combined extracts were

References:

WO2014/140077,2014,A1 Location in patent:Page/Page column 37