Reacción #1458425

Ecuación de reacción

water

diphenylphosphine sulfide

N,N-diethylchloroacetamide

potassium hydroxide

→

N,N-Diethylcarbamoylmethyl-diphenylphosphine sulfide

Disolventes

methylene chloride

Condiciones de reacción

Tratamiento posterior

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

Procedimiento

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.

Fuente