반응 #70951

ord-c05757ac7f494c32be36a5b288116313

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the solvents were evaporated to dryness
  2. 2
    기타the crude solid was triturated with diethyl ether (15 mL)
  3. 3
    여과filtered
  4. 4
    기타dried

실험 절차

A mixture of 1-(3,4-bis(benzyloxy)-5-nitrophenyl)-2-(2-(trifluoromethyl)pyridin-3-yl)ethanone (0.485 g, 0.93 mmol), ethyl carbazate (0.11 g, 1.06 mmol) and p-toluene sulfonic acid (4 mg) in toluene (10 mL) was refluxed until distillation of water ceased. The reaction mixture was cooled to room temperature, the solvents were evaporated to dryness, and the crude solid was triturated with diethyl ether (15 mL), filtered and dried yielding (Z)-ethyl 2-(1-(3,4-bis(benzyloxy)-5-nitrophenyl)-2-(2-(trifluoromethyl)pyridin-3-yl)ethylidene)hydrazinecarboxylate, 0.475 g (84%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08536203B2uspto-grants-2013_09