HRID1658114
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 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
- distillationThe dimethylsulfoxide was distilled off in vacuo
- washThe chloroform solution was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated to dryness
- customThe residual solid was recrystallized from a mixture of n-hexane and acetone
- customto yield 1.21 of the product, m.p. 208°- 210°C with decomposition