HRID1072790
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAfter evaporation of the solvent under reduced pressure, water (45 ml) and ethylenediamine (2.7 g)
- additionwere added to the residue
- temperaturethe mixture was heated at 70° C. for 15 min
- concentrationThe solution was concentrated under reduced pressure
- customthe residue was purified by a short silica gel column