반응 #49920

ord-1eddb448ff674889bf5ee66e8cf10c6f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the reaction mixture was partitioned between saturated aqueous sodium bicarbonate (20 ml) and ether (20 ml)
  2. 2
    기타The ether layer was evaporated under reduced pressure to about 10 ml
  3. 3
    기타the excess hydrazine was removed by filtration
  4. 4
    기타The filtrate was evaporated

실험 절차

N'-t-butyl-N-benzoylhydrazine (1.0 g,) in 2 ml toluene was added dropwise to a solution of beta-trifluoromethylcrotonyl chloride (prepared by addition of oxalyl chloride (1.3 g) to a solution of 1.5 g beta-trifluoromethylcrotonic acid in 5 ml toluene at 23° C.). After 30 minutes at 23° C., the reaction mixture was partitioned between saturated aqueous sodium bicarbonate (20 ml) and ether (20 ml). The ether layer was evaporated under reduced pressure to about 10 ml and the excess hydrazine was removed by filtration. The filtrate was evaporated to give N'-t-butyl-N-benzoyl-N'-(beta-trifluoromethylcrotonyl)hydrazine as a colorless oil.

출처

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