HRID1738826
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 5-(5-indanyl)-5-(pyrido[2,3-d]pyrimidin-4-yl) barbituric acid (3.734 g, 10 mM) and sodium hydroxide (2.00 g, 50 mM) in water (40 ml) is refluxed for 15 h. After cooling the solution is made slightly acidic (pH4-5) by addition of HCl and again refluxed for 15 h. The solution is cooled, made strongly basic with sodium hydroxide and then extracted with ethyl acetate. The organic phase is washed with water, dried and then evaporated to dryness under vacuum. The residue is purified by column chromatography using dichloromethane/methanol 93:7 as eluant. Thus pure title compound is obtained in about 60% yield.
WORKUP
后处理
- temperatureAfter cooling the solution
- temperatureagain refluxed for 15 h
- temperatureThe solution is cooled
- extractionextracted with ethyl acetate
- washThe organic phase is washed with water
- customdried
- customevaporated to dryness under vacuum
- customThe residue is purified by column chromatography