HRID569823

反应详情

EQUATION

反应方程式

HRID 569823 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl 2-[3-(4-bromo-2-fluorobenzyl)-7-chloro-1,2,3,4-tetrahydro-2,4-dioxoquinazolin-1-yl]-acetate (249 g) and 1N aqueous sodium hydroxide (795 ml) in methanol (1.6 l) was refluxed for 30 minutes with stirring. The solvent was evaporated and the residue was dissolved in hot water (5 l). The aqueous solution was poured into ice-cold 0.5N hydrochloric acid (3 l). The precipitates were collected by filtration and recrystallized from a mixture of ethanol (6 l) and water (3 l) to give 2-[3-(4-bromo-2-fluorobenzyl)-7-chloro-1,2,3,4-tetrahydro-2,4-dioxoquinazolin-1-yl]-acetic acid (198 g).

WORKUP

后处理

  1. temperaturewas refluxed for 30 minutes
  2. customThe solvent was evaporated
  3. dissolutionthe residue was dissolved in hot water (5 l)
  4. additionThe aqueous solution was poured into ice-cold 0.5N hydrochloric acid (3 l)
  5. filtrationThe precipitates were collected by filtration
  6. customrecrystallized from a mixture of ethanol (6 l) and water (3 l)