반응 #2191

ord-3e56139cc6e34a43b00746088801690f

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwas added
  2. 2
    온도The mixture was gradually heated to the reflux temperature
  3. 3
    workup.STIRRINGstirred for 2 hours
  4. 4
    온도under reflux
  5. 5
    workup.WAITit was left
  6. 6
    온도to cool
  7. 7
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

실험 절차

N-(4-chloro-4'-trifluoromethylsulfonylmethylbenzhydryl) -N'-methoxycarbonylhydrazine (1.6 g) was added to methanol (80 ml), and hydrochloric acid (3 ml) was added thereto with stirring at room temperature. The mixture was gradually heated to the reflux temperature and stirred for 2 hours under reflux, and then it was left to cool. The solvent was distilled off under reduced pressure to obtain the desired product as a slightly yellow powder (1.6 g, melting point: 52° to 54° C., yield: 91.5%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728699uspto-grants-1998_03