反应 #1885093

反应方程式

2,2,2-trifluoro-1-(4-o-tolyl-piperazin-1-yl)-ethanone

chlorosulfonic acid

→

product

收率 80.7%

4-Methyl-3-[4-(2,2,2-trifluoro-acetyl)-piperazin-1-yl]-benzenesulfonyl chloride

收率 80.7%

溶剂

dichloromethane

反应条件

后处理

1. 1
   其他at −5° C.
2. 2
   workup.STIRRINGthe reaction mixture continued stirring for 16 h
3. 3
   温度to warm to room temperature
4. 4
   温度After cooling to 0° C.
5. 5
   萃取The aqueous phase was extracted five times with dichloromethane
6. 6
   洗涤the combined organic phases washed with aqueous sodium bicarbonate solution and saturated sodium chloride solution
7. 7
   干燥The organic layer was dried over magnesium sulphate
8. 8
   过滤filtered
9. 9
   其他the solvent evaporated

实验过程

To a solution of 2 g of 2,2,2-trifluoro-1-(4-o-tolyl-piperazin-1-yl)-ethanone (7.35 mmol) in 5 mL of dichloromethane at −5° C. were slowly added 19.7 g of chlorosulfonic acid (169 mmol). After stirring for 2 h at −5° C., the reaction mixture continued stirring for 16 h, thereby slowly allowed to warm to room temperature. After cooling to 0° C., the reaction mixture was slowly added to a water/ice mixture. The aqueous phase was extracted five times with dichloromethane, the combined organic phases washed with aqueous sodium bicarbonate solution and saturated sodium chloride solution. The organic layer was dried over magnesium sulphate, filtered, and the solvent evaporated to yield 2.2 g of product as a white solid.

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