反应详情

Crude diethyl 2-[6,7-dichloro-2-(3-chloro-2-butenyl)-2,3-dihydro-1-oxo-2-propyl-1H-inden-5-yl]malonate (36.9 g, 0.075 mole) was refluxed with stirring in a mixture of ethanol (100 ml), water (100 ml) and sodium hydroxide (15 g) for 2 hours. The reaction mixture was cooled, diluted with water and extracted with hexane. The aqueous layer was acidified with hydrochloric acid and extracted with methylene chloride. The organic extracts were washed with water, dried over MgSO4 and concentrated under vacuum to obtain 17 g of product which after recrystallization from a mixture of methyl cyclohexane and butyl chloride melted at 111°-114° C. and was shown by HPLC to be a 95% trans, 5% cis mixture.

1. temperatureThe reaction mixture was cooled
2. extractionextracted with hexane
3. extractionextracted with methylene chloride
4. washThe organic extracts were washed with water
5. dry with materialdried over MgSO4
6. concentrationconcentrated under vacuum