HRID238086

反应详情

EQUATION

反应方程式

HRID 238086 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 7-benzyloxy-4-(4-bromo-2-fluoroanilino)-6-methoxyquinazoline hydrochloride (9.4 g, 19.1 mmol) in TFA (90 ml) was heated at reflux for 50 minutes. The mixture was allowed to cool and was poured on to ice. The resulting precipitate was collected by filtration and dissolved in methanol (70 ml). The solution was adjusted to pH9-10 with concentrated aqueous ammonia solution. The mixture was concentrated to half initial volume by evaporation. The resulting precipitate was collected by filtration, washed with water and then ether, and dried under vacuum to give 4-(4-bromo-2-fluoroanilino)-7-hydroxy-6-methoxyquinazoline (5.66 g, 82%).

WORKUP

后处理

  1. temperatureat reflux for 50 minutes
  2. temperatureto cool
  3. additionwas poured on to ice
  4. filtrationThe resulting precipitate was collected by filtration
  5. dissolutiondissolved in methanol (70 ml)
  6. concentrationThe mixture was concentrated to half initial volume
  7. customby evaporation
  8. filtrationThe resulting precipitate was collected by filtration
  9. washwashed with water
  10. dry with materialether, and dried under vacuum