HRID856736

反应详情

EQUATION

反应方程式

HRID 856736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1-methyl-3-nitro-5-[[(1-propylimidazol-5-yl)methyl]thio]-1,2,4-triazole (2.8 g) was added 85% ethanol solution (84 ml), calcium chloride (0.57 g) and reduced iron (2.9 g) were added to the mixture, and the mixture was heated to reflux for 3 hours. After cooling to room temperature, the mixture was filtered with Celite, and washed with ethyl acetate. The organic layer was washed with water and saturated brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure, and the obtained residue was purified by silica gel column chromatography, to give 1-methyl-5-[[(1-propylimidazol-5-yl)methyl]thio]-1,2,4-triazole-3-amine (0.86 g).

WORKUP

后处理

  1. additionwere added to the mixture
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 3 hours
  4. filtrationthe mixture was filtered with Celite
  5. washwashed with ethyl acetate
  6. washThe organic layer was washed with water and saturated brine
  7. dry with materialdried over magnesium sulfate
  8. customThe solvent was removed under reduced pressure
  9. customthe obtained residue was purified by silica gel column chromatography