Reaktion #1458425

Reaktionsgleichung

water

diphenylphosphine sulfide

N,N-diethylchloroacetamide

potassium hydroxide

→

N,N-Diethylcarbamoylmethyl-diphenylphosphine sulfide

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle