반응 #1458425

반응 방정식

water

diphenylphosphine sulfide

N,N-diethylchloroacetamide

potassium hydroxide

→

N,N-Diethylcarbamoylmethyl-diphenylphosphine sulfide

용매

methylene chloride

반응 조건

후처리

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

실험 절차

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.

출처