反应 #2194

反应方程式

Difluoromethyl chloride

4-chloro-4'-mercaptomethylbenzophenone

potassium hydroxide

dioxane

4-chloro-4'-mercaptomethylbenzophenone

→

desired product

收率 36.0%

4-Chloro-4'-difluoromethylthiomethyl-benzophenone

收率 36.0%

溶剂

water

反应条件

后处理

1. 1
   过滤subjected to filtration
2. 2
   干燥The organic layer as the filtrate was dried over anhydrous magnesium sulfate
3. 3
   workup.ADDITIONadd
4. 4
   浓缩concentrated
5. 5
   其他The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1)

实验过程

4-chloro-4'-mercaptomethylbenzophenone (14.7 g) and potassium hydroxide (15 g) was added to a solvent comprising dioxane (100 ml) and water (100 ml). Difluoromethyl chloride was blown into this solution at 60° C. until the starting material 4-chloro-4'-mercaptomethylbenzophenone disappeared. The reaction product was cooled to room temperature and then subjected to filtration. The organic layer as the filtrate was dried over anhydrous magnesium sulfate add concentrated. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1) to obtain the desired product (6.4 g, melting point: 34° to 35° C., yield: 36%).

来源