HRID977955

反应详情

EQUATION

反应方程式

HRID 977955 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 1-benzyl-5-(1,3-dithiol-2-ylidene)-4,6-dioxopiperidine-3-carboxylate (2.0 g) is dissolved in ethanol (160 ml), and a 10% aqueous sodium hydroxide solution (8.0 ml) is added thereto. The mixture is refluxed for 2 hours. The mixture is cooled, neutralized with 10% hydrochloric acid, and then evaporated under reduced pressure to remove the solvent. The residue is dissolved in ethyl acetate, and the solution is washed with water, dried and then evaporated to remove the solvent. The residue thus obtained is recrystallized from isopropanol, whereby 1-benzyl-3-(1,3-dithiol-2-ylidene)-2,4-dioxopiperidine (1.26 g) is obtained as pale yellow needles. Yield: 78%.

WORKUP

后处理

  1. temperatureThe mixture is refluxed for 2 hours
  2. temperatureThe mixture is cooled
  3. customevaporated under reduced pressure
  4. customto remove the solvent
  5. dissolutionThe residue is dissolved in ethyl acetate
  6. washthe solution is washed with water
  7. customdried
  8. customevaporated
  9. customto remove the solvent
  10. customThe residue thus obtained
  11. customis recrystallized from isopropanol