HRID1517416

反应详情

EQUATION

反应方程式

HRID 1517416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a suspension of 4-chloro-6-(3-methyl-4-methoxyphenyl)-pyrido[3,2-d]pyrimidine (0.99 mmole) in isopropanol (40 ml) was added piperazine (1.99 mmole). The reaction mixture was heated at 80° C. for 2 hours. The solvents were evaporated in vacuo. The crude residue was purified by silica gel flash chromatography (the mobile phase being a mixture of methanol and dichloromethane with an 0.5% aqueous NH3 solution (in a ratio gradually ranging from 2:98 to 3:97), resulting in the pure title compound (259 mg, yield 78%) which was characterized by its mass spectrum as follows: MS (m/z): 336 ([M+H]+, 100).

WORKUP

后处理

  1. customThe solvents were evaporated in vacuo
  2. customThe crude residue was purified by silica gel flash chromatography (the mobile phase
  3. additiona mixture of methanol and dichloromethane with an 0.5% aqueous NH3 solution (in a ratio