HRID1698532

反应详情

EQUATION

反应方程式

HRID 1698532 的结构方程式

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

  1. temperatureThe reaction was cooled to room temperature
  2. customquenched into 1675 mL ice water
  3. additionThe resulting slurry was adjusted to pH 9 by the addition of 125 mL saturated aqueous ammonium hydroxide
  4. filtrationThe precipitate was filtered
  5. washwashed with 200 mL water
  6. customdried in a vacuum oven at 50° C. overnight