HRID54415

反应详情

EQUATION

反应方程式

HRID 54415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a mixture of 1.25 g (5.43 mmol) of 5,6-dichloro-2,4-dihydroxyquinoline and 6,7-dichloro-2,4-dihydroxyquinoline in 8 mL of glacial acetic acid was added 1.5 mL of HNO3 (69-71%) and the mixture was heated at 90° C. for 2 h. The mixture was cooled to room temperature, filtered and washed with water, and dried to leave 280 mg (19%) of the title compound as a yellow solid, mp 235°-236° C. (decomposed). 1H NMR (CDCl3 +DMSO-d6), 7.362 (s, 1), 8.039 (s, 1), 11.369 (s, 1). MS, 274 (50, M+), 214 (100), 187 (18), 160 (20). High resolution MS, Calcd for C9H435Cl2N2O4 273.9544, found 273.9548.

WORKUP

后处理

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationfiltered
  3. washwashed with water
  4. customdried