HRID867183
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling
- customthe precipitate was collected
- washwashed with water
- dissolutionwith hot water, and dissolved in a 10% sodium hydroxide solution
- filtrationThe insoluble material was filtered off
- customThe resulting precipitate was collected
- customrecrystallized from dimethyl sulfoxide