反应详情

To a solution of the compound (3) (0.97 g, 4.5 mmol) in toluene (1.88 g) was added dropwise a solution of the compound (10a) (0.87 g, 3.2 mmol) in acetonitrile (4 ml) under ice-cooling for 30 minutes. A solution of triethylamine (0.46 g, 4.5 mmol) in acetonitrile (0.5 ml) was added dropwise thereto for 15 minutes, and the mixture was stirred under ice-cooling for 2 hours. The reaction mixture was concentrated under reduced pressure and extracted with ethyl acetate. The extract was washed with water, concentrated under reduced pressure and purified by column chromatography on silica gel (elution ethyl acetate) to yield the objective (11) (1.17 g) as a crystal. Yield 82%. Mp 133–135° C.

1. temperaturecooling for 30 minutes
2. temperaturecooling for 2 hours
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. extractionextracted with ethyl acetate
5. washThe extract was washed with water
6. concentrationconcentrated under reduced pressure
7. custompurified by column chromatography on silica gel (elution ethyl acetate)