反应详情

温度

70 °C

The sodium salt prepared in Example I (420 gm, 1.6M) is intermittently mixed with phosphorous pentachloride (160 gm, 0.77M) in a three liter multi-necked flask and slowly warmed to 70° C. in an oil bath. The liquified reaction mass is aged at 70° C. for 8 hours, then cooled to room temperature and carefully poured over one kilogram of cracked ice. A solid precipitate is removed by filtration and the aqueous phase is extracted with methylene chloride three times, each time using 300 milliliters of MeCl. The combined organic phases are dried and concentrated using a rotary evaporator. 4-cyclohexylbenzenesulfonyl chloride (338 gm, 81% of theoretical yield) was recovered as a crude product.

1. customThe liquified reaction mass
2. temperaturecooled to room temperature
3. customA solid precipitate is removed by filtration
4. extractionthe aqueous phase is extracted with methylene chloride three times
5. customThe combined organic phases are dried
6. concentrationconcentrated
7. customa rotary evaporator
8. custom4-cyclohexylbenzenesulfonyl chloride (338 gm, 81% of theoretical yield) was recovered as a crude product