تفاعل #1458425

معادلة التفاعل

water

diphenylphosphine sulfide

N,N-diethylchloroacetamide

potassium hydroxide

→

N,N-Diethylcarbamoylmethyl-diphenylphosphine sulfide

المذيبات

methylene chloride

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas cooled to 8–10° C. in an ice-water bath
2. 2
   أخرىthe organic layer was separated
3. 3
   غسيلwashed with more water (25 ml)
4. 4
   تجفيفdried over sodium sulfate
5. 5
   أخرىThe solvent was removed under reduced pressure
6. 6
   أخرىa rotary evaporator
7. 7
   أخرىthe oily residue was crystallized from ethyl acetate-hexane mixture
8. 8
   أخرىto give 3.5 g (53%) of large cubes

الإجراء التجريبي

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.

المصدر