HRID1075279

反应详情

EQUATION

反应方程式

HRID 1075279 的结构方程式

PROCEDURE

实验过程

To a solution of ethyl 2-(4-amino-6-chloropyrimidin-2-yl)acetate (21.5 g) in methanol (200 ml) was added a solution of sodium metal (7.25 g) in methanol (130 ml) and the mixture was refluxed for 3.5 hours. The reaction mixture was cooled in an ice-salt bath and saturated with dry hydrogen chloride and then allowed to stand overnight at ambient temperature. The mixture was evaporated to dryness and the residue was dissolved in a mixture of ethyl acetate and a cold aqueous solution of sodium bicarbonate. The organic layer was separated out, washed with water, dried over anhydrous magnesium sulfate and and evaporated to give methyl 2-(4-amino-6-methoxypyrimidin-2-yl)acetate (14.2 g), mp 91°-94° C.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 3.5 hours
  2. customThe mixture was evaporated to dryness
  3. dissolutionthe residue was dissolved in a mixture of ethyl acetate
  4. customThe organic layer was separated out
  5. washwashed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated