HRID1670522
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureCool to room temperature
- custom(reaction solidifies)
- filtrationFilter off the solid
- customDry the solid in vacuo