HRID1709225

反应详情

EQUATION

反应方程式

HRID 1709225 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

1.5 g (7.1 mmol) N-carboxyethyl-2-nitroaniline was dissolved in 50 ml ethanol and the solution was hydrogenated at atm. pressure by using 5% Pd/C (100 mg) as a catalyst. The reaction mixture was filtered and evaporated. 50 ml 4N hydrochloric acid and 1.6 g (13 mmol) oxalic acid dihydrate was added, and the reaction mixture was refluxed for 2 h. After cooling to 25° C. the precipitate was filtered off, washed with water and ethanol to give 0,4 g (24%) 1-carboxyethyl-quinoxaline-2,3(1H,4H)-dione. M.p. >300° C. 1H-NMR (DMSO-d6): 12.0 (1H, broad s), 7.2 (4H, m), 4.3 (2H, t), 2.6 (2H, t).

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. customevaporated
  3. temperaturethe reaction mixture was refluxed for 2 h
  4. filtrationwas filtered off
  5. washwashed with water and ethanol