반응 #667545

ord-180c1dc5fd6343a78ad341603de1d08a

시약

없음

반응 조건

온도
70°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After the exothermal reaction
  2. 2
    기타The low boilers were removed under vacuum
  3. 3
    workup.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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04752648uspto-grants-1988_06