反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customAfter the theoretical amount of hydrogen gas was absorbed
- filtrationthe catalyst was filtered off
- concentrationthe filtrate was concentrated under reduced pressure
- extractionextracted with ethyl acetate
- dry with materialThe extract was dried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residual solid was recrystallized from ethanol