反应详情

温度

0 °C

4.87 g of para-toluenesulfonyl chloride (25.5 mmol) are slowly added to a solution of 6.70 g of (4-fluoro-4-hydroxymethylpiperidin-1-yl)-(3-chloro-4-fluorophenyl)methanone (23.12 mmol) in 40 ml of pyridine cooled to 0° C. and maintained under a nitrogen atmosphere. The mixture is stirred for 12 hours at room temperature and then it is poured into ice-cold water, extracted with chloroform and then the organic phase is washed with a 1N aqueous solution of hydrochloric acid. The organic phase is dried over magnesium sulfate, filtered and then concentrated under vacuum. The title product is purified by recrystallization from a dichloromethane/diisopropyl ether mixture. 7.73 g of a white crystalline powder are obtained.

1. temperaturemaintained under a nitrogen atmosphere
2. additionit is poured into ice-cold water
3. extractionextracted with chloroform
4. washthe organic phase is washed with a 1N aqueous solution of hydrochloric acid
5. dry with materialThe organic phase is dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under vacuum
8. customThe title product is purified by recrystallization from a dichloromethane/diisopropyl ether mixture