HRID658996

反应详情

EQUATION

反应方程式

HRID 658996 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringthe mixture stirred for 12 h at r.t
  2. stirringthe mixture stirred for 5 d at r.t
  3. customThe reaction mixture was evaporated
  4. customthe residue was purified by chromatography on silica gel (dichloromethane/methanol 95:5)
  5. washThe obtained material was washed with ether
  6. dissolutiondissolved in hot ethanol
  7. customevaporated
  8. customAfter treatment with a small amount of ethanol the precipitate was isolated by filtration
  9. customdried