HRID489281

反应详情

EQUATION

反应方程式

HRID 489281 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-hydroxynicotinic acid methyl ester (3-067-02) (20 g) in methylene chloride (500 mL) was added N-iodosuccinimide (NIS, 38 g) at room temperature, and the reaction mixture was heated under reflux for 16 h, and evaporated. To the residue was added ethyl acetate (200 mL) and the reaction mixture was heated under reflux for 2 h. The insoluble solid was filtered to give 2-hydroxy-5-iodonicotinic acid methyl ester (3-067-03) (30 g, 81%) as a white solid.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 16 h
  3. customevaporated
  4. additionTo the residue was added ethyl acetate (200 mL)
  5. temperaturethe reaction mixture was heated
  6. temperatureunder reflux for 2 h
  7. filtrationThe insoluble solid was filtered