反应 #1458425

反应方程式

water

diphenylphosphine sulfide

N,N-diethylchloroacetamide

potassium hydroxide

→

N,N-Diethylcarbamoylmethyl-diphenylphosphine sulfide

溶剂

methylene chloride

反应条件

后处理

1. 1
   温度was cooled to 8–10° C. in an ice-water bath
2. 2
   其他the organic layer was separated
3. 3
   洗涤washed with more water (25 ml)
4. 4
   干燥dried over sodium sulfate
5. 5
   其他The solvent was removed under reduced pressure
6. 6
   其他a rotary evaporator
7. 7
   其他the oily residue was crystallized from ethyl acetate-hexane mixture
8. 8
   其他to give 3.5 g (53%) of large cubes

实验过程

A stirred mixture of diphenylphosphine sulfide (4.365 g, 0.02 mol) and N,N-diethylchloroacetamide (4.189 g, 0.028 mol) in methylene chloride (80 ml) was cooled to 8–10° C. in an ice-water bath. Small pieces of solid potassium hydroxide (3.927 g, 0.07 mol) were added while stirring under nitrogen atmosphere. After 30 minutes, water (25 ml) was added and the organic layer was separated, washed with more water (25 ml) and dried over sodium sulfate. The solvent was removed under reduced pressure using a rotary evaporator and the oily residue was crystallized from ethyl acetate-hexane mixture to give 3.5 g (53%) of large cubes. mp: 108–110° C.

来源