反应详情

To a 0° C. solution of 10 g (55 mmoles) of 3-hydroxy-4-p-fluorophenoxy-1-butyne (Example 157) in 75 ml of dry dimethylformamidee and 88 g (130 mmoles) of imidazole is added dropwise, with stirring, 7.5 g (68 mmoles) of chlorotrimethylsilane. The mixture, while under an argon atmosphere, is stirred at room temperature for 18 hours, and then poured into 150 ml of hexane and 100 ml of ice-water. Thhe organic phase is separated, washed with 50 ml of a brine solution, dried with magnesium sulfate, and evaporated under vacuum. This crude product is distilled under vacuum at 0.1 mm (bp 73°-75° C.), to give 12.2 g (91%) of the subject compound as a colorless oily liquid.

1. stirringThe mixture, while under an argon atmosphere, is stirred at room temperature for 18 hours
2. customThhe organic phase is separated
3. washwashed with 50 ml of a brine solution
4. dry with materialdried with magnesium sulfate
5. customevaporated under vacuum
6. distillationThis crude product is distilled under vacuum at 0.1 mm (bp 73°-75° C.)