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
In 2 mL of dichloromethane, 608 mg (2.12 mmol) of 3-(methylpiperazin-1-ylmethyl)-5-(trifluoromethyl)aniline was dissolved, and 380 mg (2.34 mmol) of 1,1′-carbonylbis-1H-imidazole was added there to under cooling with ice, and the mixture solution was stirred at room temperature for three hours. To the reaction solution, 520 mg (2.16 mmol) of [9-(4-aminophenyl)-9H-purin-6-yl]-methylamine and 4 ml of dimethylformamide were added, and the mixture solution was further stirred at 40° C. for four hours. The residue obtained by concentrating the reaction solution was partitioned between water and ethyl acetate, and the organic layer was washed with a saturated sodium chloride solution and concentrated under reduced pressure. The product was recrystallized from ethyl acetate to obtain 742 mg (62%) of a target product as a white crystal.
WORKUP
后处理
- temperatureto under cooling with ice
- stirringthe mixture solution was further stirred at 40° C. for four hours
- customThe residue obtained
- concentrationby concentrating the reaction solution
- customwas partitioned between water and ethyl acetate
- washthe organic layer was washed with a saturated sodium chloride solution
- concentrationconcentrated under reduced pressure
- customThe product was recrystallized from ethyl acetate