HRID1599036

反应详情

EQUATION

反应方程式

HRID 1599036 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (2-methoxyphenoxy)malonic acid diethyl ester (10.0 g) and thiourea (4.04 g) in methanol (100 ml) is added dropwise with stirring a 28% solution of sodium methoxide in methanol (17.07 g) over a period of 30 minutes under ice-cooling. The mixture is stirred at room temperature overnight. After the reaction is completed, the mixture is evaporated under reduced pressure to remove the solvent, and water (200 ml) is added to the residue. To the mixture is further added methyl iodide (3.30 ml), and the mixture is reacted at room temperature for three hours. The reaction solution is acidified with 10% aqueous hydrochloric acid, and the precipitated crystals are collected by filtration, washed with water, and dried to give 4,6-dihydroxy-5-(2-methoxyphenoxy)-2-methylthiopyrimidine (8.90 g).

WORKUP

后处理

  1. temperaturecooling
  2. customthe mixture is evaporated under reduced pressure
  3. customto remove the solvent, and water (200 ml)
  4. additionis added to the residue
  5. customthe mixture is reacted at room temperature for three hours
  6. filtrationthe precipitated crystals are collected by filtration
  7. washwashed with water
  8. customdried