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温度

0 °C

Under a nitrogen atmosphere 2,3-dihydro-4,5-dimethoxy-1H-inden-1-one (31.7 g) was dissolved in 600 ml of anhydrous 1,2-dichloroethane and cooled to 0° C. Aluminum chloride (44 g) was added in portions and the reaction mixture was heated to 60° C. for 17 hours, cooled to room temperature and poured into ice/water. After extraction with dichloromethane the organic layer was dried and evaporated. The residue was crystallized from ethyl acetate to give 20.5 g of 2,3-dihydro-4-hydroxy-5-methoxy-1H-inden-1-one, M.S. (C.I.) (M/Z): 179 [M+H]+.

1. temperaturethe reaction mixture was heated to 60° C. for 17 hours
2. temperaturecooled to room temperature
3. extractionAfter extraction with dichloromethane the organic layer
4. customwas dried
5. customevaporated
6. customThe residue was crystallized from ethyl acetate