Dicyclohexylphosphine → Chlorodicyclohexylphosphine
반응식
[CH:1]1([PH:7][CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.P(Cl)(Cl)(Cl)(Cl)[Cl:15]>C1(C)C=CC=CC=1>[CH:8]1([P:7]([CH:1]2[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]2)[Cl:15])[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13]1참가 물질
4
실험 절차
A solution of 19 g (0.1 mol) dicyclohexylphosphine in 50 ml toluene was dropped into a suspension of 21 g (0.1 mol) PCl5 in 100 ml toluene. The reaction temperature was maintained at less than 30° C. After all had been dropped in, the whole was boiled for 1 hour under reflux. A slight precipitate was removed by means of a reverse frit and the reaction mixture was freed from all low boilers at 60° C. under 0.1 mbar. Yield: 23.3 g; 31P-NMR: δ P=126 ppm, (c-C6H11)2PCl, 96 mol %; δ P=54 ppm, (c-C6H11)2P(O)Cl, 3.7 mol %.
후처리
- temperatureThe reaction temperature was maintained at less than 30° C
- additionAfter all had been dropped in, the whole
- temperatureunder reflux
- customA slight precipitate was removed by means of a reverse frit
- customwas freed from all low boilers at 60° C. under 0.1 mbar
출처 및 근거
- ORD 기록
- ord-3c747dcb9a764531aa7d598f1c5b78dd
- 출처 데이터셋
- uspto-grants-1988_06
- 특허 번호
- US04752648
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