反応 #1458425

反応方程式

water

diphenylphosphine sulfide

N,N-diethylchloroacetamide

potassium hydroxide

→

N,N-Diethylcarbamoylmethyl-diphenylphosphine sulfide

溶媒

methylene chloride

反応条件

後処理

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

実験手順

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.

出典