HRID1698532
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 135 °C
PROCEDURE
实验过程
A solution of 20.0 g (103 mmol) 3-methyl-4-nitro-1H-imidazo[4,5-c]pyridin-2(3H)-one in 168 mL 48% hydrobromic acid was heated for 6 h at 135° C. An additional 33 mL of 48% hydrobromic acid was added and the reaction was stirred at 135° C. overnight. The reaction was cooled to room temperature and quenched into 1675 mL ice water. The resulting slurry was adjusted to pH 9 by the addition of 125 mL saturated aqueous ammonium hydroxide. The precipitate was filtered and washed with 200 mL water and dried in a vacuum oven at 50° C. overnight to give 17.58 g (75%) of the title product as a light yellow solids.
WORKUP
后处理
- temperatureThe reaction was cooled to room temperature
- customquenched into 1675 mL ice water
- additionThe resulting slurry was adjusted to pH 9 by the addition of 125 mL saturated aqueous ammonium hydroxide
- filtrationThe precipitate was filtered
- washwashed with 200 mL water
- customdried in a vacuum oven at 50° C. overnight