反应详情

温度

0 °C

Dropwise 13 ml (0.17 mole) of methanesulfonyl chloride was added to a solution of 28.9 g (0.1 mole) of 3-hydroxy-1-[4-chloro-2-(2-fluorobenzoyl)phenyl]propyne and 24.4 ml (0.175 mole) of triethylamine in 300 ml of methylene chloride which was cooled to 0° C. The mixture was washed with ice water, cold 1N hydrochloric acid, cold saturated aqueous sodium bicarbonate and dried over anhydrous sodium sulfate. Concentration of the methylene chloride solution gave a brown oil which was crystallized from ether to give a yellow solid. Recrystallization from a mixture of ether and petroleum ether gave off-white prisms, mp 95°-96° C.

1. washThe mixture was washed with ice water, cold 1N hydrochloric acid, cold saturated aqueous sodium bicarbonate
2. dry with materialdried over anhydrous sodium sulfate
3. customConcentration of the methylene chloride solution gave a brown oil which
4. customwas crystallized from ether
5. customto give a yellow solid
6. customRecrystallization
7. additionfrom a mixture of ether and petroleum ether
8. customgave off-white prisms, mp 95°-96° C.