HRID353825

反应详情

EQUATION

反应方程式

HRID 353825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. dissolutionAfter all of the solid had dissolved the reaction solution
  2. customThe dichloromethane was removed under vacuum
  3. additionA catalytic amount of sodium isopropoxide was added to the solution
  4. temperaturethe solution was heated
  5. temperatureat reflux for 1 hour
  6. concentrationThe solution was then concentrated under vacuum
  7. extractionextracted with diethyl ether
  8. dry with materialThe extract was dried over magnesium sulfate
  9. concentrationconcentrated under vacuum