反应详情

126 mg (0.625 mmol) of 4-hydroxy-piperidine-1-carboxylic acid tert-butyl ester were dissolved in 2.5 mL of dimethylacteamide and 30 mg (0.75 mmol) of NaH (60% purity) were added at room temperature. After 15 minutes 181 mg (0.5 mmol) of 7-bromo-6-fluoro-2-(4-methoxy-benzyl)-2H-isoquinolin-1-one (313) were added and stirring was continued at room temperature. After 5.5 h the solvent was removed i. vac. After adding saturated sodium bicarbonatesodium bicarbonate solution, the mixture was extracted twice with dichloromethane. The organic layers were dried with MgSO4 and evaporated. After final purification by preparative HPLC, 182 mg of the product could be isolated. Rt=1.93 min (Method C). Detected mass: 543.5/545.5 (M+H+).

1. customwas continued at room temperature
2. customAfter 5.5 h the solvent was removed i
3. additionAfter adding saturated sodium bicarbonatesodium bicarbonate solution
4. extractionthe mixture was extracted twice with dichloromethane
5. dry with materialThe organic layers were dried with MgSO4
6. customevaporated
7. customAfter final purification by preparative HPLC, 182 mg of the product
8. customcould be isolated