HRID543137

反应详情

EQUATION

反应方程式

HRID 543137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureheated
  2. temperatureunder reflux for 20 hours
  3. customThe solvent was evaporated
  4. customthe residue was partitioned between ethyl acetate and water
  5. customThe organic layer was separated
  6. washwashed with 2N hydrochloric acid
  7. customto remove any unreacted amine
  8. washIt was then washed with water
  9. customdried
  10. filtrationfiltered
  11. customevaporated
  12. customto give a yellow gum
  13. washChromatography on silica "Kieselgel 60H" (Trade Mark) eluting with ethyl acetate