HRID1059293

反应详情

EQUATION

反应方程式

HRID 1059293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

1.60 g of 4-[(3-chloropyrazin-2-yl)thio]-3-nitrobenzyl alcohol was dissolved in a solvent mixture of tetrahydrofuran (20 ml)/2-propanol (20 ml)/water (7 ml). After adding 0.16 g of ammonium chloride and 1.50 g of iron powder, the resulting mixture was heated under reflux for 30 minutes. Then the reaction mixture was filtered through celite and concentrated under reduced pressure. After adding ethanol, the reaction mixture was concentrated under reduced pressure. Then tetrahydrofuran was added to the residue and the insoluble matters were separated by filtration. After distilling off the solvent under reduced pressure, 1.47 g of the title compound was obtained as yellow crystals.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 30 minutes
  3. filtrationThen the reaction mixture was filtered through celite and
  4. concentrationconcentrated under reduced pressure
  5. additionAfter adding ethanol
  6. concentrationthe reaction mixture was concentrated under reduced pressure
  7. additionThen tetrahydrofuran was added to the residue
  8. customthe insoluble matters were separated by filtration
  9. distillationAfter distilling off the solvent under reduced pressure