反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
205.6 mg (1.268 mmol) 1,1′-Carbonyl-diimidazol (CDI) were given to a solution of 220.3 mg (1.153 mmol) 2-methoxy-5-(trifluoromethyl)aniline in 4.0 ml dichloromethane. After stirring for 2 h a formed precipitate was dissolved by addition of 5 ml THF and the mixture stirred for 12 h at r.t. A solution of 300.0 mg (1.153 mmol) 3-[4-(4-Amino-phenoxy)-pyrimidin-2-ylamino]-propan-1-ol in 6 ml dichloromethane was added and the mixture stirred for 5 d at r.t. The reaction mixture was evaporated and the residue was purified by chromatography on silica gel (dichloromethane/methanol 95:5). The obtained material was washed with ether and dissolved in hot ethanol and evaporated. After treatment with a small amount of ethanol the precipitate was isolated by filtration and dried. Yield: 172 mg (31%) of the title compound.
WORKUP
后处理
- stirringthe mixture stirred for 12 h at r.t
- stirringthe mixture stirred for 5 d at r.t
- customThe reaction mixture was evaporated
- customthe residue was purified by chromatography on silica gel (dichloromethane/methanol 95:5)
- washThe obtained material was washed with ether
- dissolutiondissolved in hot ethanol
- customevaporated
- customAfter treatment with a small amount of ethanol the precipitate was isolated by filtration
- customdried