Реакция #1458425

Уравнение реакции

water

diphenylphosphine sulfide

N,N-diethylchloroacetamide

potassium hydroxide

→

N,N-Diethylcarbamoylmethyl-diphenylphosphine sulfide

Растворители

methylene chloride

Условия реакции

Обработка

1. 1
   Температураwas cooled to 8–10° C. in an ice-water bath
2. 2
   Другоеthe organic layer was separated
3. 3
   Промывкаwashed with more water (25 ml)
4. 4
   Сушкаdried over sodium sulfate
5. 5
   ДругоеThe solvent was removed under reduced pressure
6. 6
   Другоеa rotary evaporator
7. 7
   Другоеthe oily residue was crystallized from ethyl acetate-hexane mixture
8. 8
   Другоеto give 3.5 g (53%) of large cubes

Методика

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.

Источник