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
PROCEDURE
实验过程
2-[2-Aminoethoxymethyl]-3-ethoxycarbonyl-4-(2-chlorophenyl)-5-methoxycarbonyl-6-methyl-1,4-dihydropyridine (0.75 g) and 2-methylthio-3H-pyrimid-4-one (0.5 g) were dissolved in ethanol (5 ml) and heated under reflux for 20 hours. The solvent was evaporated and the residue was partitioned between ethyl acetate and water. The organic layer was separated, washed with 2N hydrochloric acid to remove any unreacted amine, and then with dilute sodium hydroxide solution. It was then washed with water, dried, filtered and evaporated to give a yellow gum. Chromatography on silica "Kieselgel 60H" (Trade Mark) eluting with ethyl acetate gave the title compound, which was recrystallised from ethyl acetate, yield 171 mg, m.p. 148°-150°.
WORKUP
后处理
- temperatureheated
- temperatureunder reflux for 20 hours
- customThe solvent was evaporated
- customthe residue was partitioned between ethyl acetate and water
- customThe organic layer was separated
- washwashed with 2N hydrochloric acid
- customto remove any unreacted amine
- washIt was then washed with water
- customdried
- filtrationfiltered
- customevaporated
- customto give a yellow gum
- washChromatography on silica "Kieselgel 60H" (Trade Mark) eluting with ethyl acetate