HRID1765345

反应详情

EQUATION

反应方程式

HRID 1765345 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

To a solution of 7-Amino-2-Isopropyl-4-bromo-2H-phthalazin-1-one (0.8 g, 0.0028 mol) in DMF (8 ml), was added potassium carbonate (2 g, 0.014 mol). After five minutes, bis (2-chloroethyl)ether (0.41 g, 0.0028 mol) was added and the solution was heated to 140° C. for 24 hours. After this time LC-MS indicated the complete consumption of starting material and the mixture was cooled, concentrated under vacuum and purified by flash column chromatography (elution: 70% heptane, 30% ethyl acetate) to give the title compound (0.2 g, 20% yield) as a white solid.

WORKUP

后处理

  1. customthe complete consumption of starting material
  2. temperaturethe mixture was cooled
  3. concentrationconcentrated under vacuum
  4. custompurified by flash column chromatography (elution: 70% heptane, 30% ethyl acetate)