HRID556268
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
- 120 °C
PROCEDURE
实验过程
A solution of 6-bromo-2-methoxy-pyridin-3-ylamine (1A) (5.2 g, 25.6 mmol) in acetic acid (50 mL) and HBr (50 mL) is heated to reflux with an oil bath at 120° C. for 1 hour. The reaction solution is cooled to room temperature and concentrated to dryness. The crude product is purified by chromatography (CH2Cl2 95%, MeOH 5%) to give 3-amino-6-bromo-1H-pyridin-2-one (1B) (3.5 g, yield 72%) as brown solid that turns to deep purple. MS (ESI) m/e 189, 191 (M+H+).
WORKUP
后处理
- temperatureThe reaction solution is cooled to room temperature
- concentrationconcentrated to dryness
- customThe crude product is purified by chromatography (CH2Cl2 95%, MeOH 5%)