HRID346133

反应详情

EQUATION

反应方程式

HRID 346133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 10.5 g (31.7 mmol) 2-cyano-5-ethoxalylamino-4-nitrobenzotrifluoride in 450 ml ethanol was added 45 ml glacial acetic acid. The mixture was hydrogenated at atm. pressure by using 0.2 g 5% Pd-C as a catalyst. The filtered and evaporated reaction product was recrystallized (ethylacetate-light petroleum) to give 6.91 g (81%) of 7-cyano-1-hydroxy-6-trifluoromethyl-quinoxaline-2,3(1H,4H)-dione. M.p. 180° C. decomp. 1H-NMR (DMSO-d6): 7.93 (1H, s), 7.53 (1H, s). MS (m/e): 271 (M+, 70%).

WORKUP

后处理

  1. filtrationThe filtered
  2. customevaporated
  3. customreaction product
  4. customwas recrystallized (ethylacetate-light petroleum)