反应详情

To a solution of compound 65 (3 g, 11 mmol) and acrylonitrile (3.2 mL, 51 mmol) in absolute CH3OH (50 mL) was added a catalytic amount of CH3ONa (71 mg, 1.32 mmol) at room temperature with stirring under N2. The mixture was stirred at room temperature for overnight under N2. The mixture was diluted with aqNaHCO3 and extracted with DCM. The combined organic layers were washed with brine, dried over Na2SO4, concentrated and purified with silica gel column chromatography (PE:EtOAc=5:1) to give compound 66 (1.9 g, 64%) as a light yellow solid.

1. stirringThe mixture was stirred at room temperature for overnight under N2
2. additionThe mixture was diluted with aqNaHCO3
3. extractionextracted with DCM
4. washThe combined organic layers were washed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated
7. custompurified with silica gel column chromatography (PE:EtOAc=5:1)