反应详情

温度

80 °C

To 2a,3,4,5-tetrahydro-2H-acenaphthylen-1-one oxime (7.00 g) was added a solution (about 65%, 50 ml) of sodium bis(2-methoxyethoxy)aluminum dihydride in toluene, and the mixture was stirred with heating at 80° C. for 2 hr. After cooling to room temperature, the reaction mixture was poured into ice water, and the mixture was extracted with chloroform. After concentration under reduced pressure, the residue was extracted with 1N hydrochloric acid. The aqueous layer was alkalified with potassium carbonate, and extracted with chloroform. The extract was washed with saturated brine, dried over sodium sulfate, and concentrated under reduced pressure to give the title compound (5.34 g, 83%).

1. temperatureAfter cooling to room temperature
2. extractionthe mixture was extracted with chloroform
3. concentrationAfter concentration under reduced pressure
4. extractionthe residue was extracted with 1N hydrochloric acid
5. extractionextracted with chloroform
6. washThe extract was washed with saturated brine
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated under reduced pressure