HRID1670522

反应详情

EQUATION

反应方程式

HRID 1670522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Mix 6-hydroxy-nicotinic acid (14 g, 101 mmol) and pyridine (0.41 mL, 0.49 mmol) in acetonitrile (60 mL). Heat the mixture at 80° C. for 30 min. Add thionyl chloride (7.6 mL, 104 mmol) and continue heating at 80° C. for an additional 1.5 h. Cool to room temperature (reaction solidifies). Filter off the solid using a minimal amount of cold acetonitrile. Dry the solid in vacuo to obtain the desired intermediate as a tan solid (11.2 g, 70%).

WORKUP

后处理

  1. temperatureCool to room temperature
  2. custom(reaction solidifies)
  3. filtrationFilter off the solid
  4. customDry the solid in vacuo