HRID4691

反应详情

EQUATION

反应方程式

HRID 4691 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-acetyl-6-(2-dimethylaminoethyl)-4-(3-nitrophenyl)-2-phenylpyrimidine (1 g) and sodium borohydride (0.1 g) in methanol (40 ml) was stirred for 1 hour. The reaction mixture was poured into a mixture of water and chloroform and adjusted the pH to 9. The extract was dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel eluting with a mixture of chloroform and methanol (20:1). The fractions containing the desired product were combined and concentrated in vacuo. The residue was recrystallized from diethyl ether to afford 6-(2-dimethylaminoethyl)-5-(1-hydroxyethyl)-4-(3-nitrophenyl)-2-phenylpyrimidine (0.2 g).

WORKUP

后处理

  1. dry with materialThe extract was dried over magnesium sulfate
  2. customevaporated in vacuo
  3. customThe residue was chromatographed on silica gel eluting with a mixture of chloroform and methanol (20:1)
  4. additionThe fractions containing the desired product
  5. concentrationconcentrated in vacuo
  6. customThe residue was recrystallized from diethyl ether