HRID2287362

反应详情

EQUATION

反应方程式

HRID 2287362 的结构方程式

PROCEDURE

实验过程

Sodium (181 mg) was dissolved in 10 ml of methanol and 400 mg of N-[6-chloro-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide was added with stirring at room temperature. The reaction mixture was stirred at room temperature for three hours and poured into a mixture of 1N hydrochloric acid and ice. The crystals separated out therefrom were collected by filtration and the resulting crystals were purified by a silica gel column chromatography (chloroform-methanol=40:1). The resulting yellow amorphous substance was crystallized in ether and collected by filtration to give 273 mg of N-[6-methoxy-5-(2-methoxyphenoxy)-2-(2-pyrimidinyl)-4-pyrimidinyl]-2-phenylethenesulfonamide.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred at room temperature for three hours
  2. customThe crystals separated out
  3. filtrationtherefrom were collected by filtration
  4. customthe resulting crystals were purified by a silica gel column chromatography (chloroform-methanol=40:1)
  5. customThe resulting yellow amorphous substance was crystallized in ether
  6. filtrationcollected by filtration