反应详情

1 g of 9-methoxymethyl-9-hydroxymethyl-fluorene (4.2 mmol) was dissolved in 20 ml of dichloromethane. The solution was cooled in ice-water bath, and 0.7 ml of triethyl amine (5 mmol) was added thereto. After stirring for 5 minutes, 0.6 ml of trimethylsilyl chloride (4.6 mmol) was added drop-wise, and the mixture was stirred for further 2 hours, followed by stirring at room temperature for 1 hour. The reaction mixture was washed with water, and the organic layer separated was dried over anhydrous sodium sulfate. After filtration, the filtrate was evaporated to give 1.41 g of concentrate (yield 86%). MS(EI)m/e: 312(M+).

1. stirringthe mixture was stirred for further 2 hours
2. stirringby stirring at room temperature for 1 hour
3. washThe reaction mixture was washed with water
4. customthe organic layer separated
5. dry with materialwas dried over anhydrous sodium sulfate
6. filtrationAfter filtration
7. customthe filtrate was evaporated
8. customto give 1.41 g
9. concentrationof concentrate (yield 86%)