反应详情

温度

55 °C

To a solution of Part E compound (600 mg, 2.45 mmol) in DMF (20 mL) was added Example 2 Part A compound (2-(4-piperidinyl)-2,3-dihydro-1H-isoindol-1-one) (530 mg, 2.45 mmol) followed by anhydrous potassium carbonate (372 mg, 2.69 mmol). The reaction was stirred at 55° C. overnight. The reaction was cooled to RT. Ethyl ether (200 mL) was added to dilute the reaction, and the organic layer was washed with water (2×50 mL), brine (2×50 mL) and dried over MgSO4. Evaporation gave a crude oil. Purification was performed by flash chromatography on 100 g of silica gel, loaded and eluted with 2% methanol in dichloromethane. Pure fractions were combined and evaporated to give a colorless oil. The resulting oil was dissolved in methanol (2 mL) and HCl in ethyl ether solution (1.0 M, 3.0 mL, 3.0 mmol) was added. The HCl salt precipitated from the solution. The salt was filtered and dried at 60° C. under vacuum to give title compound (490 mg, 80%) as a white solid.

1. temperatureThe reaction was cooled to RT
2. additionto dilute
3. customthe reaction
4. washthe organic layer was washed with water (2×50 mL), brine (2×50 mL)
5. dry with materialdried over MgSO4
6. customEvaporation
7. customgave a crude oil
8. customPurification
9. washeluted with 2% methanol in dichloromethane
10. customevaporated
11. customto give a colorless oil
12. customThe HCl salt precipitated from the solution
13. filtrationThe salt was filtered
14. customdried at 60° C. under vacuum