HRID1658114

反应详情

EQUATION

反应方程式

HRID 1658114 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture containing 1.0 g of ethyl 2-chloro-5,8-dihydro-8-ethyl-5-oxopyrido[2,3-d]pyrimidine-6-carboxylate, 0.60 g of sodium bicarbonate, 20 ml of dimethyl sulfoxide, and 0.60 g of 1-acetylpiperazine was heated at 120°C for 1.5 hours with stirring. The dimethylsulfoxide was distilled off in vacuo and the residue was taken up in chloroform. The chloroform solution was washed with water, dried over anhydrous magnesium sulfate, and concentrated to dryness. The residual solid was recrystallized from a mixture of n-hexane and acetone to yield 1.21 of the product, m.p. 208°- 210°C with decomposition.

WORKUP

后处理

  1. distillationThe dimethylsulfoxide was distilled off in vacuo
  2. washThe chloroform solution was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated to dryness
  5. customThe residual solid was recrystallized from a mixture of n-hexane and acetone
  6. customto yield 1.21 of the product, m.p. 208°- 210°C with decomposition