反应详情

To a stirred solution of (rac)-4-(8-amino-5,6,7,8-tetrahydroisoquinolin-4-yl)benzonitrile (example 1) (480 mg, 1.93 mmol) and propionic acid (158 μL, 2.12 mmol) in CH2Cl2 (10 mL) at 0° C. under Argon was added EDCI (406 mg, 2.12 mmol). Stirring was continued over night and the reaction mixture was allowed to warm up to room temperature. The reaction mixture was poured into aq. 10% KH2PO4 solution followed by extraction with AcOEt (3×). The organic phases were washed once with aq. 10% KH2PO4, aq. sat. NaHCO3 and with aq. sat. NaCl solution. The combined organic phases were dried over Na2SO4, filtered and evaporated to afford the title compound (558 mg, 95%) as light brown solid. MS: 306.2 (M+H+).

1. waitwas continued over night
2. extractionfollowed by extraction with AcOEt (3×)
3. washThe organic phases were washed once with aq. 10% KH2PO4, aq. sat. NaHCO3 and with aq. sat. NaCl solution
4. dry with materialThe combined organic phases were dried over Na2SO4
5. filtrationfiltered
6. customevaporated