반응 #90296

ord-bf696df99e3c42e4bef874a61be84a2e

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: US09446012B2uspto-grants-2016_09