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-dimethylamino-6-morpholino-1,3,5-triazine 492mg (2.02 mmol) was dissolved in DMF (20 ml), added with sodium hydroxide (182 mg, 4.55 mmol) and imidazole (308 mg, 4.52 mmol) and stirred at 110° C.-120° C. for 45 minutes. The reaction mixture was evaporated under reduced pressure. The residue obtained was added with dichloromethane and water, and then was 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 residue was purified by silica gel column chromatography, using dichloromethane and methanol (95:5) as eluant, to obtain 508 mg (yield: 91.4%) of the titled compound as colorless crystals.
WORKUP
后处理
- customThe reaction mixture was evaporated under reduced pressure
- customThe residue obtained
- stirringwas shaken
- 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 residue was purified by silica gel column chromatography