반응 #667545
ord-180c1dc5fd6343a78ad341603de1d08a
시약
없음
반응 조건
온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타After the exothermal reaction
- 2기타The low boilers were removed under vacuum
- 3workup.DISTILLATIONThe residue was distilled under vacuum
실험 절차
38.5 g (0.34 mol) phenylphosphine dissolved in 40 ml toluene was added at 25° C. to a suspension of 160 g PCl5 (0.77 mol) in 500 ml toluene. After the exothermal reaction had subsided, the whole was heated to 70° C. until gas ceased to be evolved. The low boilers were removed under vacuum. The crude product yield was 67 g; 31P-NMR: δ P=161 ppm, C6H5PCl2, 94.4 mol%. The residue was distilled under vacuum. bp 98° C./17 mbar; yield: 50.6 g (81% of the theoretical).