HRID42227

反应详情

EQUATION

反应方程式

HRID 42227 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Furan-2,3-dicarboxylic acid dimethyl ester (1.6 g, 8.69 mmol) is added to EtOH (10 mL) and hydrazine hydrate (1.46 mL, 55% in water). Heat the reaction to reflux for 5-6 h. Cool and concentrate in vacuo to form a slurry. Dilute the material with additional H2O and filter the precipitate. Wash with additional H2O. Transfer material from filter to a round bottom flask and add HCl (7.2 mL, 2N in H2O). Heat reaction mixture to reflux for 4 h. Cool and filter the precipitate washing with H2O, to yield the title compound without further purification (930 mg, 70%)

WORKUP

后处理

  1. temperatureHeat
  2. customthe reaction
  3. temperatureto reflux for 5-6 h
  4. temperatureCool
  5. concentrationconcentrate in vacuo
  6. customto form a slurry
  7. filtrationfilter the precipitate
  8. washWash with additional H2O
  9. filtrationTransfer material from filter to a round bottom flask
  10. additionadd HCl (7.2 mL, 2N in H2O)
  11. temperatureHeat
  12. customreaction mixture
  13. temperatureto reflux for 4 h
  14. temperatureCool
  15. filtrationfilter the precipitate
  16. washwashing with H2O