반응 #1725593

반응 방정식

trichlorosilane

(2S,4S)-4-dicyclohexylphosphinyl-2-diphenylphosphinylmethylpyrrolidine

triethylamine

→

title compound

수율 95.0%

(2S,4S)-4-dicyclohexylphosphino-2-diphenylphosphinomethylpyrrolidine

수율 95.0%

용매

acetonitrile

acetonitrile

반응 조건

후처리

1. 1
   온도cooling
2. 2
   온도After refluxing the mixture for 3 hours
3. 3
   농축the mixture was concentrated under reduced pressure at a low temperature
4. 4
   workup.DISSOLUTIONThe residual product was dissolved in 15 ml of benzene
5. 5
   workup.ADDITION10 ml of a 30% aqueous solution of caustic soda was added to the benzene solution under ice-
6. 6
   온도cooling
7. 7
   기타The benzene phase was separated
8. 8
   추출the aqueous phase was extracted with 10 ml of benzene
9. 9
   세척washed with 10 ml of water
10. 10
    건조dried over magnesium sulfate

실험 절차

In 4 ml of acetonitrile were dissolved 50 mg (0.1 m-mol) of (2S,4S)-4-dicyclohexylphosphinyl-2-diphenylphosphinylmethylpyrrolidine [X] and 42 mg (0.42 m-mol) of triethylamine, and the air in the reaction vessel was satisfactorily replaced with nitrogen. A solution of 54 mg (0.4 m-mol) of trichlorosilane in 1 ml of acetonitrile was added dropwise to the above solution under ice-cooling. After refluxing the mixture for 3 hours, the mixture was concentrated under reduced pressure at a low temperature. The residual product was dissolved in 15 ml of benzene, and 10 ml of a 30% aqueous solution of caustic soda was added to the benzene solution under ice-cooling. The mixture was stirred in nitrogen atmosphere for 30 minutes at 50°60° C. The benzene phase was separated and the aqueous phase was extracted with 10 ml of benzene. The benzene phases are combined, washed with 10 ml of water, dried over magnesium sulfate and concentrated under reduced pressure whereby 44 mg (yield: 95%) of the title compound was obtained.

출처