HRID1924071

反应详情

EQUATION

反应方程式

HRID 1924071 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

A mixture of 5-nitrothiophene-2-carboxylic acid (5.000 g, 28.9 mmol) in SOCl2 (40 mL) was refluxed for 2 h. The excess SOCl2 was evaporated in vacuo and 3-amino-4-hydroxypyridine (2.65 g, 24.1 mmol) in pyridine (150 mL) was added dropwise. The reaction mixture was stirred at 10° C. overnight. Na2CO3 (1.533 g, 14.5 mmol) in water (100 mL) was added and the resultant mixture was stirred for additional 1 h. The precipitate was collected by filtration, washed with 10% Na2CO3 (120 mL), and dried in vacuo to afford N-(4-hydroxypyridin-3-yl)-5-nitrothiophene-2-carboxamide as a yellow powder (5.87 g, yield: 92%).

WORKUP

后处理

  1. temperaturewas refluxed for 2 h
  2. additionwas added dropwise
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with 10% Na2CO3 (120 mL)
  5. customdried in vacuo