反应详情

温度

0 °C

Trifluoroacetic acid (1.15 g, 10.1 mmol) was added to a solution of 2-(3,4-dichloro-phenylamino)-N-(2,2-dimethoxy-ethyl)-N-(3-piperidin-1-yl-propyl)-propionamide (300 mg, 0.67 mmol) in CH2Cl2 (6 mL) at 0° C. After 30 min the ice bath was removed, then after 1 h triethylsilane (391 mg, 3.36 mmol) was added. After 16 h the reaction mixture was cooled to 0° C. and treated with triethylamine, then after 15 min partitioned between CH2Cl2 and sat. aq. NaHCO3 solution. The organic layer was washed with brine, dried (MgSO4), and evaporated. Chromatography (IST Isolute® Flash NH2; EtOAc) afforded the title compound (184 mg, 71%). Yellow oil, MS: 384.2 (M+H)+.

1. customAfter 30 min the ice bath was removed
2. customafter 15 min partitioned between CH2Cl2 and sat. aq. NaHCO3 solution
3. washThe organic layer was washed with brine
4. dry with materialdried (MgSO4)
5. customevaporated