반응 #555005

ord-0b7f42c6d6d5439da1e9827d5f87c50a

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was heated
  2. 2
    온도to reflux for 18 h
  3. 3
    기타The 1,2-dimethoxyethane was removed under reduced pressure
  4. 4
    기타the residual solid was recrystallized from 1-chlorobutane
  5. 5
    기타The solid was isolated by filtration
  6. 6
    기타dried

실험 절차

To a solution of 2-amino-3-bromo-5-(trifluoromethyl)pyridine (10.0 g, 41.5 mmol) in 1,2 dimethoxyethane (300 mL) at room temperature was added ethyl bromopyruvate (9.889 g, 45.64 mmol) dropwise. The reaction mixture was heated to reflux for 18 h. The 1,2-dimethoxyethane was removed under reduced pressure and the residual solid was recrystallized from 1-chlorobutane. The solid was isolated by filtration and dried to afford an off-white solid, 8-bromo-6-(trifluoromethyl)imidazo[1,2-a]pyridine-2-carboxylic acid, ethyl ester (11.044 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08623890B2uspto-grants-2014_01