HRID2290335

反应详情

EQUATION

反应方程式

HRID 2290335 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-Methyl-3-(1-methylhydrazino)-6-phenyl-1,2,4-triazine (2.9 g) was dissolved in ethanol (50 ml) containing anhydrous hydrogen chloride and hydrogenated over 5% palladium on carbon (0.33 g) under atmospheric pressure at room temperature. After the theoretical amount of hydrogen gas was absorbed, the catalyst was filtered off, and the filtrate was concentrated under reduced pressure. The residue was neutralized with an aqueous solution of sodium carbonate and extracted with ethyl acetate. The extract was dried over sodium sulfate and concentrated under reduced pressure. The residual solid was recrystallized from ethanol to give colorless crystals of 5-methyl-3-(1-methylhydrazino)-6-phenyl-2,5-dihydro-1,2,4-triazine, mp 139.5°~141° C.

WORKUP

后处理

  1. customAfter the theoretical amount of hydrogen gas was absorbed
  2. filtrationthe catalyst was filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. extractionextracted with ethyl acetate
  5. dry with materialThe extract was dried over sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residual solid was recrystallized from ethanol