반응 #2493

ord-86e31c9534414a65b91ab486505f6497

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated
  2. 2
    기타The reaction solution is subsequently evaporated to dryness at 12 torr/40° C
  3. 3
    추출extracted twice with 30 ml of water each time
  4. 4
    건조The organic phase is dried over sodium sulfate
  5. 5
    기타evaporated to dryness at 12 torr/40° C

실험 절차

4 g (7.3 mmol) of 4,4-diphenyl-4,5-dihydro-3H-dinaphtho-[2,1-c:1',2'-e]phosphepinium bromide are suspended in a mixture of 80 ml of 2N sodium hydroxide solution and 30 ml of ethanol and heated to boiling for 4 hours. The reaction solution is subsequently evaporated to dryness at 12 torr/40° C. The residue is taken up in 80 ml of dichloromethane and extracted twice with 30 ml of water each time. The organic phase is dried over sodium sulfate and evaporated to dryness at 12 torr/40° C. This gives colorless crystals (melting point: 199.5° C.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728886uspto-grants-1998_03