Reacción #2194

Ecuación de reacción

Difluoromethyl chloride

4-chloro-4'-mercaptomethylbenzophenone

potassium hydroxide

dioxane

4-chloro-4'-mercaptomethylbenzophenone

→

desired product

Rendimiento 36.0%

4-Chloro-4'-difluoromethylthiomethyl-benzophenone

Rendimiento 36.0%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Filtraciónsubjected to filtration
2. 2
   SecadoThe organic layer as the filtrate was dried over anhydrous magnesium sulfate
3. 3
   workup.ADDITIONadd
4. 4
   Concentraciónconcentrated
5. 5
   OtroThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=5:1)

Procedimiento

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%).

Fuente