반응 #49948

ord-9570592e9f8441c1bc76aa768282e77a

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타producing a mild exotherm
  2. 2
    기타The reaction was quenched 2 minutes later with water (20 ml) and ether (20 ml)
  3. 3
    기타separated
  4. 4
    세척the organic washed with 0.1N HCl
  5. 5
    건조dried over MgSO4
  6. 6
    여과filtered

실험 절차

Methyl dichlorophosphine (1.3 g) in ether (10 ml) and triethylamine (2 ml) were added to a stirred solution of N-benzoyl-N'-t-butyl hydrazine (1.0 g) in methylene chloride (3 ml). After stirring 5 minutes at room temperature, o-chloroaniline was added neat producing a mild exotherm. The reaction was quenched 2 minutes later with water (20 ml) and ether (20 ml), separated and the organic washed with 0.1N HCl, dried over MgSO4, filtered and rotavapped to a colorless oil weighing 0.5 g.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05424333uspto-grants-1995_06