HRID1789583

反应详情

EQUATION

反应方程式

HRID 1789583 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 1,4-dihydro-2-methoxy-6-methyl-4-(3-nitrophenyl)-5-pyrimidinecarboxylic acid, ethyl ester (3.19 g, 10.0 mmoles) in dichloromethane (25 ml) and pyridine (5.0 ml) under argon was cooled to 0° C. and was treated dropwise with ethyl chloroformate (1.2 ml of 0.7%, 12.0 mmoles). After the addition was completed, the reaction was allowed to warm to room temperature and stirred for 1 hour. It was then diluted with ethyl acetate and the resulting solution was washed with water, sodium bicarbonate and brine. After drying over anhydrous magnesium sulfate, the solvent was evaporated to provide 2-methoxy-4-methyl-6-(3-nitrophenyl)-1,5(6H)-pyrimidinedicarboxylic acid, diethyl ester as a light yellow foam (3.71 g). This material was used in the next reaction without purification.

WORKUP

后处理

  1. additionAfter the addition
  2. washthe resulting solution was washed with water, sodium bicarbonate and brine
  3. dry with materialAfter drying over anhydrous magnesium sulfate
  4. customthe solvent was evaporated