HRID2422676

反应详情

EQUATION

反应方程式

HRID 2422676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4-Methoxy-3-nitropyridine-2-carboxylic acid (1.35 g, 6.81 mmol), sodium hydrogencarbonate (690 mg, 817 mmol), water (10 mL) and 10% palladium-carbon (135 mg) were stirred in a hydrogen atmosphere at room temperature for 24 hours. The reaction solution was filtered through Celite, the Celite was washed with water and methanol, and the mother liquid was concentrated. 2 N hydrochloric acid was added to the resulting residue, and the solution was controlled to have a pH of 1. The reaction solution was stirred at 0° C. for 1 hour, and the resulting pale gray solid was taken out through filtration and dried to obtain the intended compound (940 mg, 56%).

WORKUP

后处理

  1. filtrationThe reaction solution was filtered through Celite
  2. washthe Celite was washed with water and methanol
  3. concentrationthe mother liquid was concentrated
  4. addition2 N hydrochloric acid was added to the resulting residue
  5. filtrationthe resulting pale gray solid was taken out through filtration
  6. customdried