HRID444434

反应详情

EQUATION

反应方程式

HRID 444434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 17.7 g. of 4,5-dichloro-o-phenylenediamine and 200 ml. of anhydrous ethanol was prepared. A 17.4 g. batch of diethyl 2-keto-malonate was added to this solution and the mixture was heated to refluxing temperature for about 17 hours. The volatile constituents were removed by evaporation in vacuo. Recrystallization of the residue from ethanol yielded 20 g. of ethyl 6,7-dichloro-3,4-dihydro-3-oxo-2-quinoxaline carboxylate formed in the above reaction; melting in the range of 226°-227° C.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto refluxing temperature for about 17 hours
  3. customThe volatile constituents were removed by evaporation in vacuo
  4. customRecrystallization of the residue from ethanol
  5. customyielded 20 g