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
PROCEDURE
实验过程
Carbonyl diimidazole (18.6 g, 0.115 mol) was added to a suspension of 6-chloronicotinic acid (16.6 g, 0.105 mol) in dichloromethane (250 mL). After all of the solid had dissolved the reaction solution was stirred at ambient temperature for 1 hour and then isopropyl alcohol (100 mL) was added. The dichloromethane was removed under vacuum. A catalytic amount of sodium isopropoxide was added to the solution and the solution was heated at reflux for 1 hour. The solution was then concentrated under vacuum. The resulting residue was slurried with water and then extracted with diethyl ether. The extract was dried over magnesium sulfate and then concentrated under vacuum to provide 23.9 g of isopropyl 6-chloronicotinate.
WORKUP
后处理
- dissolutionAfter all of the solid had dissolved the reaction solution
- customThe dichloromethane was removed under vacuum
- additionA catalytic amount of sodium isopropoxide was added to the solution
- temperaturethe solution was heated
- temperatureat reflux for 1 hour
- concentrationThe solution was then concentrated under vacuum
- extractionextracted with diethyl ether
- dry with materialThe extract was dried over magnesium sulfate
- concentrationconcentrated under vacuum