HRID490091
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
- 180 °C
PROCEDURE
实验过程
To a solution of 5-bromo-N-(4-methoxybenzyl)-3-methylindazole 105 (0.12 g, 0.363 mmol) in NMP (N-methylpyrrolidinone; 2 mL) was added sodium cyanide (0.035 g, 0.714 mmol) and nickel bromide (0.079 g, 0.362 mmol). The reaction mixture was heated in a microwave reactor at 180° C. for 20 minutes. Ethyl acetate (100 mL) was added and the organic layer was washer with water and brine. The organic layer was dried over sodium sulfate. The organic solvent was evaporated under reduced pressure. The crude product was purified by flash column chromatography to yield the desired 5-cyano-N-(4-methoxybenzyl)-3-methylindazole 106 (0.1 g, 0.361 mmol).
WORKUP
后处理
- dry with materialThe organic layer was dried over sodium sulfate
- customThe organic solvent was evaporated under reduced pressure
- customThe crude product was purified by flash column chromatography