HRID350654

反应详情

EQUATION

反应方程式

HRID 350654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 3-hydroxypicolinate (2.0 g) was dissolved in 100 ml of acetone. Potassium carbonate (3.4 g) and 3.4 ml of benzyl bromide were added to the solution, and a reaction was allowed to proceed at room temperature overnight. The reaction solution was then refluxed for 4 hr. Water (50 ml) was added thereto, and the mixture was neutralized with 1 N hydrochloric acid, followed by concentration under the reduced pressure. Methylene chloride and water were added to the residue. The organic layer was dried over magnesium sulfate, and was then dried under the reduced pressure. The dried organic layer was then purified by column chromatography (chloroform-methanol) to give 2.1 g (yield 62%) of methyl 3-benzyloxypicolinate.

WORKUP

后处理

  1. temperatureThe reaction solution was then refluxed for 4 hr
  2. concentrationfollowed by concentration under the reduced pressure
  3. additionMethylene chloride and water were added to the residue
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. customwas then dried under the reduced pressure
  6. customThe dried organic layer was then purified by column chromatography (chloroform-methanol)