Réaction #1458425

Équation de réaction

water

diphenylphosphine sulfide

N,N-diethylchloroacetamide

potassium hydroxide

→

N,N-Diethylcarbamoylmethyl-diphenylphosphine sulfide

Solvants

methylene chloride

Conditions de réaction

Traitement

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

Mode opératoire

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.

Source