反应详情

温度

80 °C

106 mg (4.20 mmol) of sodium hydride (95%) were suspended in 3 mL of dimethyl acetamide and 193 mg (1.40 mmol) of (1S,3S)-3-amino-cyclopentanol (34), dissolved in 1 mL of dimethyl acetamide, were added dropwise. After 1 h, 402 mg (1.42 mmol) of 2-(4-methoxy-benzyl)-6-fluoro-2H-isoquinolin-1-one (9), dissolved in another 3 mL of dimethyl acetamide, were added. The reaction mixture was stirred at 80° C. until the reaction was complete. The mixture was poured into water, extracted three times with a mixture of dichloromethane and 2-propanol (3:1) and the combined organic layers were evaporated. Water was added and the crude product was subjected to lyophilization to remove remainders of dimethyl acetamide. The obtained crude product was purified by silica gel chromatography to yield 250 mg of the title compound (39). Rt=1.20 min (Method E). Detected mass: 365.2 (M+H+).

1. additionwere added dropwise
2. additionwere added
3. extractionextracted three times
4. additionwith a mixture of dichloromethane and 2-propanol (3:1)
5. customthe combined organic layers were evaporated
6. additionWater was added
7. customto remove remainders of dimethyl acetamide
8. customThe obtained crude product
9. customwas purified by silica gel chromatography