HRID1413795

反应详情

EQUATION

反应方程式

HRID 1413795 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 2-(3-chloro-4-bromobenzyl)-1,2-dihydro-1-oxophthalazin-4-ylacetate (7.0 g.) in ethanol (70 ml.) containing potassium hydroxide (7.0 g.) was heated under reflux for 30 minutes. The solution was then poured into water (250 ml.) and the aqueous solution was extracted with ether (2×150 ml.). The aqueous phase was acidified to pH 2 with concentrated hydrochloric acid. The solid which was thus precipitated was separated, washed with water, dried in vacuo and then recrystallised from a 6:2:3 v/v/v mixture of toluene, propan-2-ol and petrol (60-80) to give 2-(3-chloro-4-bromobenzyl)-1,2-dihydro-1-oxophthalazin-4-ylacetic acid (3.9 g.), m.p. 186° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 30 minutes
  3. extractionthe aqueous solution was extracted with ether (2×150 ml.)
  4. customThe solid which was thus precipitated
  5. customwas separated
  6. washwashed with water
  7. customdried in vacuo
  8. customrecrystallised from a 6:2:3 v/v/v mixture of toluene, propan-2-ol and petrol (60-80)