HRID54399

反应详情

EQUATION

反应方程式

HRID 54399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 102 mg (0.418 mmol) of 4,5-bis(trifluoromethyl)-1,2-phenylenediamine and 37 mg (0.411 mmol) of oxalic acid in 2 mL of 2N HCl was refluxed for 6 h and cooled to room temperature. The mixture was filtered and washed by water, CHCl3 and dried to leave a colorless solid (43 mg, 35%), mp>250° C. 1H NMR (DMSO-d6), 7.629 (s, 2) 12.293 (s, 2). 19F NMR (DMSO-d6), 62.185 (s).

WORKUP

后处理

  1. temperaturewas refluxed for 6 h
  2. filtrationThe mixture was filtered
  3. washwashed by water, CHCl3
  4. customdried