反応 #2200

反応方程式

4-chloro-4'-ethane sulfonylmethylbenzhydrol

thionyl chloride

toluene

→

desired product

収率 75.0%

4-Chloro-4'-ethane Sulfonylmethylbenzhydryl Chloride

収率 75.0%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   温度gradually heated
2. 2
   workup.STIRRINGThe mixture was stirred for 4 hours
3. 3
   温度under reflux
4. 4
   workup.WAITleft
5. 5
   温度to cool
6. 6
   workup.DISTILLATIONThen, the solvent was distilled off under reduced pressure
7. 7
   その他The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

実験手順

4-chloro-4'-ethane sulfonylmethylbenzhydrol (6.0 g), thionyl chloride (5.4 g), toluene (200 ml) and a catalytic amount of N,N-dimethylformamide were mixed and gradually heated with stirring to a refluxing temperature. The mixture was stirred for 4 hours under reflux and then left to cool. Then, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1) to obtain the desired product as a slight yellow viscous substance (4.6 g, nD20 : 1.6044, yield: 75%).

出典