HRID326976

反应详情

EQUATION

反应方程式

HRID 326976 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A solution of 5.4 g (0.02 mol) of the product from Example 1 in 10 ml of methylene chloride is added dropwise to 2.9 g (0.02 mol) of 2-amino-4-chloro-6-methylpyrimidine in 50 ml of methylene chloride at 0° C. The mixture is subsequently stirred at 25° C. for 24 hours and diluted with 50 ml of methylene chloride, and the organic phase is washed twice with 50 ml of 2N hydrochloric acid each time and once with water. After drying with sodium sulfate and removing the solvent on a rotary evaporator, an oily product remains, which crystallizes on trituration with diisopropylether. 7.8 g (91% of theory of methyl 2-[3-(4-chloro-6-methylpyrimidin-2-yl)-ureidosulfonyloxy]-3-methoxybenzoate of melting point 140°-143° C. are obtained.

WORKUP

后处理

  1. washthe organic phase is washed twice with 50 ml of 2N hydrochloric acid each time
  2. dry with materialAfter drying with sodium sulfate
  3. customremoving the solvent
  4. customon a rotary evaporator
  5. customwhich crystallizes on trituration with diisopropylether