HRID2290334

反应详情

EQUATION

反应方程式

HRID 2290334 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-methyl-3-methylthio-6-phenyl-1,2,4-triazine (20 g) and methylhydrazine (15.3 g) in ethanol (30 ml) was heated under reflux for 66 hours. After cooling, the reaction mixture was concentrated under reduced pressure and the residue was dissolved in chloroform. The solution was washed with water and brine successively, dried over sodium sulfate, and then evaporated. The residue was crystallized with diethyl ether, washed with diethyl ether, and dried to give 5-methyl-3-(1-methylhydrazino)-6-phenyl-1,2,4-triazine (13.91 g).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 66 hours
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture was concentrated under reduced pressure
  5. dissolutionthe residue was dissolved in chloroform
  6. washThe solution was washed with water and brine successively
  7. dry with materialdried over sodium sulfate
  8. customevaporated
  9. customThe residue was crystallized with diethyl ether
  10. washwashed with diethyl ether
  11. customdried