HRID1368238

反应详情

EQUATION

反应方程式

HRID 1368238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Palladium acetate (1.18 g), 1,3-bis(diphenylphosphino)propane (2.31 g) and 5-bromo-2-methyl-1H-imidazo[4,5-b]pyridine (3.72 g) were charged in an autoclave, and N,N-dimethylformamide (18.6 ml), methanol (14.9 ml) and triethylamine (5.4 ml) were added. The mixture was stirred at 85° C. for 14 hr in a 10 atm. carbon monoxide atmosphere. The reaction mixture was allowed to cool and the solvent was evaporated. Methanol (60 ml) was added to the residue and heated, and the insoluble matter was filtered off while hot. The filtrate was concentrated to give methyl 2-methyl-1H-imidazo[4,5-b]pyridine-5-carboxylate (2.95 g) as a white powder.

WORKUP

后处理

  1. additionwere added
  2. temperatureto cool
  3. customthe solvent was evaporated
  4. additionMethanol (60 ml) was added to the residue
  5. temperatureheated
  6. filtrationthe insoluble matter was filtered off while hot
  7. concentrationThe filtrate was concentrated