반응 #74897

ord-a9f0f356524647c6b03873227f24f8d3

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과filtered
  2. 2
    세척The filtrate was washed with water, dilute bicarbonate and brine
  3. 3
    건조dried over MgSO4
  4. 4
    기타Evaporation of the solvent
  5. 5
    기타afforded a yellow oil that solidified
  6. 6
    기타This crude product was recrystallized from CHCl3 /hexane

실험 절차

To a stirred solution of 1.0 g (0.004 mol) of Compound 2 in 50 ml of chloroform was gradually added 2.0 g (0.010 mol) of 85% m-chloroperbenzoic acid. The reaction mixture was stirred overnight at room temperature and then filtered. The filtrate was washed with water, dilute bicarbonate and brine, and dried over MgSO4. Evaporation of the solvent afforded a yellow oil that solidified on standing. This crude product was recrystallized from CHCl3 /hexane and a second crop of crystals was recrystallized from methanol for a total yield of 0.3 g (28% yield) of yellow crystals, m.p. 139°-141° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04174394uspto-grants-1979_11