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
The obtained 2-chloro-4-(1-imidazolyl)-6-dimethylamino-1,3,5-triazine (113 mg, 0.503 mmol) was dissolved in DMF (1 ml), added with 1,2,4-triazole (149 mg, 2.15 mmol) and stirred at 110° C.-120° C. for 4 hours. The reaction mixture was evaporated under reduced pressure. The obtained residue was added with ethyl acetate and water, and then shaken for mixing. The organic layer was separated from the mixture, washed with water and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure and the obtained residue was purified by silica gel column chromatography, using ethyl acetate and methanol (9:1) as eluant, to obtain 22.7 mg (yield: 17.6%) of the titled compound as colorless crystals.
WORKUP
后处理
- customThe reaction mixture was evaporated under reduced pressure
- additionThe obtained residue was added with ethyl acetate and water
- stirringshaken
- additionfor mixing
- customThe organic layer was separated from the mixture
- washwashed with water
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was removed under reduced pressure
- customthe obtained residue was purified by silica gel column chromatography