反应详情

To a solution of 1,1-dimethylethyl (2S)-2-methyl-1-piperazinecarboxylate (2.79 g, 13.91 mmol, supplier Antlantic Scitech) in DCM (80 mL), DIPEA (3.64 mL, 20.87 mmol) was added under argon atmosphere at room temperature then 4-cyano-2-methylbenzenesulfonyl chloride (3 g, 13.91 mmol) was added at 0° C. The ice bath was removed and the reaction mixture was stirred overnight. The reaction mixture was partitioned between DCM (30 ml) and aqueous sodium bicarbonate (2×20 ml). The organic phase was washed with HCl (2×20 ml) and water (2×20 ml) then it was dried (phase separator) and concentrated under vacuum to give the title compound (5.5 g) as a yellow viscous liquid.

1. customThe ice bath was removed
2. customThe reaction mixture was partitioned between DCM (30 ml) and aqueous sodium bicarbonate (2×20 ml)
3. washThe organic phase was washed with HCl (2×20 ml) and water (2×20 ml)
4. customit was dried (phase separator)
5. concentrationconcentrated under vacuum