反应详情

168 mg (0.83 mmol) 4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester were dissolved in 5 mL of dimethylacetamide and 20 mg (0.83 mmol) of sodium hydride (60%) were added. The mixture was stirred at room temperature. After 30 minutes a solution of 240 mg (0.67 mmol) 6-fluoro-2-(4-methoxy-benzyl)-7-phenyl-2H-iso-quinolin-1-one (315) in 5 mL of dimethylacetamide was added and stirring was continued at room temperature. After standing overnight, 20 mg (0.83 mmol) of sodium hydride (60%) were added and the solution was stirred at 100° C. After 1 h, the solvent was removed i. vac. and saturated sodium bicarbonate solution was added. The aqueous phase was extracted three times with dichloromethane. The organic layers were dried with MgSO4 and evaporated. The crude product was purified by preparative HPLC. Rt=1.98 min (Method C). Detected mass: 541.7 (M+H+).

1. stirringstirring
2. customwas continued at room temperature
3. stirringthe solution was stirred at 100° C
4. waitAfter 1 h
5. customthe solvent was removed i
6. additionand saturated sodium bicarbonate solution was added
7. extractionThe aqueous phase was extracted three times with dichloromethane
8. dry with materialThe organic layers were dried with MgSO4
9. customevaporated
10. customThe crude product was purified by preparative HPLC