HRID634722

反应详情

EQUATION

反应方程式

HRID 634722 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)-7-methoxyacetamidoquinazoline (201 mg, 0.5mmol) in methanol (5 ml) and 2M aqueous sodium hydroxide solution (0.5 ml) was stirred at ambient temperature for 1 hour. The mixture was diluted with water and adjusted to pH6 with 2M hydrochloric acid. The precipitated solid was collected by filtration, washed with water, dried and then dissolved in a mixture of methylene chloride and methanol. A 5M solution of hydrogen chloride in isopropanol (0.3 ml) was added and most of the solvent removed by evaporation. The precipitated solid was collected by filtration, washed with methylene chloride and dried under vacuum to give 4-(2-fluoro-5-hydroxy-4-methylanilino)-7-methoxyacetamidoquinazoline hydrochloride (70 mg, 36%) as a yellow solid.

WORKUP

后处理

  1. filtrationThe precipitated solid was collected by filtration
  2. washwashed with water
  3. customdried
  4. dissolutiondissolved in a mixture of methylene chloride and methanol
  5. additionA 5M solution of hydrogen chloride in isopropanol (0.3 ml) was added and most of the solvent
  6. customremoved by evaporation
  7. filtrationThe precipitated solid was collected by filtration
  8. washwashed with methylene chloride
  9. customdried under vacuum