HRID2113613

反应详情

EQUATION

反应方程式

HRID 2113613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Heat a solution of [2-chloromethyl-7-(3-trifluoromethyl-pyridin-2-yl)-quinazolin-4-yl]-(4-t-butyl-phenyl)-amine (417 mg, 0.89 mmol), Ag2O (308 mg, 1.33 mmol), and dibenzylphosphate (370 mg, 1.33 mmol) in acetonitrile at 70° C. for 18 hours. Dilute with additional acetonitrile and filter the hot solution through celite. Concentrate under reduced pressure to give a foam. Crystallize the crude product by dissolving in ether and slowly adding hexanes. Cool the resulting mixture on ice and collect the resulting solid via filtration to afford pure product.

WORKUP

后处理

  1. filtrationfilter the hot solution through celite
  2. concentrationConcentrate under reduced pressure
  3. customto give a foam
  4. customCrystallize the crude product
  5. dissolutionby dissolving in ether
  6. temperatureCool the resulting mixture on ice
  7. customcollect the resulting solid
  8. filtrationvia filtration
  9. customto afford pure product