HRID443494

反应详情

EQUATION

反应方程式

HRID 443494 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.47 g 1-(2-aminophenyl)-5-hydroxy-1H-pyrazole-4-carboxylic acid, ethyl ester and 1.78 g 1,1'-thiocarbonyl-bis-[1H-imidazole] are dissolved in 50 ml tetrahydrofuran and heated for 8 hours. The residue, after distilling off the solvent, is recrystallized from dimethylformamide to yield 2.45 g of 5,6-dihydro-1-oxo-5-thioxo-1H-pyrazolo[1,2-a][1,2,4]benzotriazine-2-carboxylic acid, ethyl ester having a melting point of 277°-282° C.; yellow needles.

WORKUP

后处理

  1. temperatureheated for 8 hours
  2. distillationThe residue, after distilling off the solvent
  3. customis recrystallized from dimethylformamide