反应 #2200616

反应方程式

5-bromo-2-(4-methyl-imidazol-1-yl)-benzonitrile

→

compound

5-Bromo-2-(5-dimethylaminomethyl-4-methyl-imidazol-1-yl)-benzonitrile

溶剂

DMF

反应条件

后处理

1. 1
   其他The solvent was evaporated
2. 2
   其他the oily residue was partitioned between saturated aqueous sodium bicarbonate solution and Ethyl acetate
3. 3
   干燥The organic phase was dried over sodium sulfate
4. 4
   浓缩concentrated
5. 5
   其他purified by chromatography (SiO2, gradient CH2Cl2 to 35% (CH2Cl2/MeOH=9/1)

实验过程

A solution of 5-bromo-2-(4-methyl-imidazol-1-yl)-benzonitrile (11.0 g, 42.0 mmol) and N,N-dimethylmethyleneiminium chloride (5.0 g, 53.4 mmol) in DMF (75 mL) was stirred at 90° C. for 16 h. The solvent was evaporated, and the oily residue was partitioned between saturated aqueous sodium bicarbonate solution and Ethyl acetate. The organic phase was dried over sodium sulfate, concentrated and purified by chromatography (SiO2, gradient CH2Cl2 to 35% (CH2Cl2/MeOH=9/1) to afford the tide compound as an oil that solidifies on standing (10.62 g, 79%). MS: m/e=319.2/321.3 [M+H]+.

来源