反应详情

To NaBH4 (0.79 g, 20.84 mmol) in THF (20 mL) at 0° C. was added TFA (2.38 g, 20.84 mmol) dropwise. To this cooled mixture was added 4-[(2-Chloro-phenyl)-cyano-methyl)-piperazine-1-carboxylic acid tert-butyl ester (101) (1.40 g, 4.17 mmol) in THF (10 mL) dropwise. The reaction mixture was allowed to stir at room temperature for 18 h. The reaction was quenched with H2O (50 mL) and diluted with EtOAc (100 mL). The organic phase was washed with H2O (100 mL) and brine (100 mL). The crude material was purified by chromatography (silica gel 60 mesh, eluting with 10% TEA/10% MeOH in EtOAc) yielding 0.49 g (34%) pure product.

1. customThe reaction was quenched with H2O (50 mL)
2. additiondiluted with EtOAc (100 mL)
3. washThe organic phase was washed with H2O (100 mL) and brine (100 mL)
4. customThe crude material was purified by chromatography (silica gel 60 mesh, eluting with 10% TEA/10% MeOH in EtOAc)