HRID279546

反应详情

EQUATION

反应方程式

HRID 279546 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-chloro-2-fluoroanilino)-6-methoxyquinazoline hydrochloride (892 mg, 2 mmol) in TFA (10 ml) was heated at reflux for 50 minutes. The mixture was allowed to cool and then poured on to ice. The precipitate was collected by filtration, dissolved in methanol (10 ml) and basified to pH11 with aqueous ammonia. The mixture was concentrated by evaporation, the resulting solid product was collected by filtration, washed with water then ether and dried under vacuum to give 4-(4-chloro-2-fluoroanilino)-7-hydroxy-6-methoxyquinazoline (460 mg, 72%) as a yellow solid.

WORKUP

后处理

  1. temperatureat reflux for 50 minutes
  2. temperatureto cool
  3. additionpoured on to ice
  4. filtrationThe precipitate was collected by filtration
  5. dissolutiondissolved in methanol (10 ml)
  6. concentrationThe mixture was concentrated by evaporation
  7. filtrationthe resulting solid product was collected by filtration
  8. washwashed with water
  9. dry with materialether and dried under vacuum