HRID2290353

反应详情

EQUATION

反应方程式

HRID 2290353 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 3-[2-(N-ethoxycarbonylglycyl)hydrazino]-5-methyl-6-phenyl-1,2,4-triazine (1.815 g) in ethanol (32 ml) containing anhydrous hydrogen chloride was shaken with 5% palladium on carbon (0.4 g) under atmosphere of hydrogen gas at room temperature. After the theoretical amount of hydrogen gas was absorbed, the catalyst was filtered off, and the filtrate was evaporated. The residue was dissolved in water and made alkaline with an aqueous solution of sodium bicarbonate under ice cooling. The resulting precipitates were collected by filtration, washed with water, dried, and recrystallized from ethanol to give colorless crystals of 3-[2-(N-ethoxycarbonylglycyl)hydrazino]-5-methyl-6-phenyl-2,5-dihydro-1,2,4-triazine (1.198 g), m.p. 144.5°~145.5° C.

WORKUP

后处理

  1. customAfter the theoretical amount of hydrogen gas was absorbed
  2. filtrationthe catalyst was filtered off
  3. customthe filtrate was evaporated
  4. dissolutionThe residue was dissolved in water
  5. customThe resulting precipitates
  6. filtrationwere collected by filtration
  7. washwashed with water
  8. customdried
  9. customrecrystallized from ethanol