HRID1957119

反应详情

EQUATION

反应方程式

HRID 1957119 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,3-diamino-5,6-dichlorotoluene (21.6 g, 0.137 mol) and oxalic acid (18.45 g, 0.206 mol) in hydrochloric acid (4M, 900 mL) was heated at reflux for 6 hours, cooled and filtered. The dark brown solid was suspended in diethyl ether, filtered and washed with more ether to give 1,4-dihydro-6,7-dichloro-5-methyl-quinoxaline-2,3-dione (22.06 g, 66%). 1H NMR (300 MHz, DMSO) 2.40 (3H, s), 7.14 (1H, s), 11.37 (1H, s), 11.94 (1H, s).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 6 hours
  3. temperaturecooled
  4. filtrationfiltered
  5. filtrationfiltered
  6. washwashed with more ether