HRID1072790

反应详情

EQUATION

反应方程式

HRID 1072790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a solution of 5-bromo-2-methyl-1H-imidazo[4,5-b]pyridine (1.92 g) in N,N-dimethylformamide (48 ml) was added Copper (I) cyanide (2.04 g), and the mixture was stirred for 9 hr at 150° C. After evaporation of the solvent under reduced pressure, water (45 ml) and ethylenediamine (2.7 g) were added to the residue, and the mixture was heated at 70° C. for 15 min. The solution was concentrated under reduced pressure and the residue was purified by a short silica gel column to give the objective compound (927 mg) as a brown powder. Purification by silica gel column chromatography (dichloromethane/methanol=10/1) gave a purer compound.

WORKUP

后处理

  1. customAfter evaporation of the solvent under reduced pressure, water (45 ml) and ethylenediamine (2.7 g)
  2. additionwere added to the residue
  3. temperaturethe mixture was heated at 70° C. for 15 min
  4. concentrationThe solution was concentrated under reduced pressure
  5. customthe residue was purified by a short silica gel column