反应详情

A water (1.0 ml) solution of CAN (336 mg, 0.613 mmols) was dropwise added to an acetonitrile (2.0 ml) solution of ethyl 8-(4,5,6,7-tetramethoxyindan-2-yl)octanoate (100 mg, 0.245 mmols) with cooling with ice and stirring was continued for 15 minutes. Water was added to the reaction mixture, which was then extracted with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution, and then dried. The solvent was evaporated in vacuo, and the resulting crude product was purified by silica gel column chromatography (hexane:ethyl acetate=8:1) followed by recrystallization from hexane to obtain the entitled compound (15 mg) as crystals.

1. temperaturewith cooling with ice
2. extractionwas then extracted with ethyl acetate
3. washThe organic layer was washed with a saturated aqueous sodium chloride solution
4. customdried
5. customThe solvent was evaporated in vacuo
6. customthe resulting crude product was purified by silica gel column chromatography (hexane:ethyl acetate=8:1)
7. customfollowed by recrystallization from hexane