HRID443493

反应详情

EQUATION

反应方程式

HRID 443493 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

24.7 g 1-(2-aminophenyl)-5-hydroxy-1H-pyrazole-4-carboxylic acid, ethyl ester and 16.2 g 1,1'-carbonyl-bis-[1H-imidazole] are dissolved in 300 ml tetrahydrofuran and stirred for 8 hours at room temperature and one hour at 90° C. The solid residue, after distilling off the solvent, is recrystallized from dimethylformamide to yield 21 g of 5,6-dihydro-1,5-dioxo-1H-pyrazolo[1,2-a][1,2,4]-benzotriazine-2-carboxylic acid, ethyl ester having a melting point of 269°-271° C.; white-yellow crystals.

WORKUP

后处理

  1. distillationThe solid residue, after distilling off the solvent
  2. customis recrystallized from dimethylformamide