HRID867183

反应详情

EQUATION

反应方程式

HRID 867183 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A suspension of ethyl 5,8-dihydro-2-(4-acetyl-1-piperazinyl)-5-oxopyrido[2,3-d]pyrimidine-6-carboxylate (20 g) in a mixture of 4% hydrochloric acid (60 ml) and ethanol (20 ml) was refluxed at 120° C. for 1.5 hours. After cooling, the precipitate was collected, washed with water and then with hot water, and dissolved in a 10% sodium hydroxide solution. The insoluble material was filtered off and the filtrate was acidified with diluted hydrochloric acid. The resulting precipitate was collected and recrystallized from dimethyl sulfoxide to give 5,8-dihydro-2-(4-acetyl-1-piperazinyl)-5-oxopyrido[2,3-d]pyrimidine-6-carboxylic acid (10 g). m.p. 298°-300° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe precipitate was collected
  3. washwashed with water
  4. dissolutionwith hot water, and dissolved in a 10% sodium hydroxide solution
  5. filtrationThe insoluble material was filtered off
  6. customThe resulting precipitate was collected
  7. customrecrystallized from dimethyl sulfoxide