HRID522613

反应详情

EQUATION

反应方程式

HRID 522613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a 500 mL round-bottom flask a mixture of 3-aminopyrazole (ALDRICH, 10 g, 120 mmol) and phthalic anhydride (ALDRICH, 24.96 g, 168 mmol) in 1,4-dioxane (150 mL) was stirred at reflux for 17 h. Solvent was evaporated to dryness. Residue was triturated with EtOH to afford (23.6 g, 111 mmol, yield 92%) of the title compound. 1H NMR (300 MHz, DMSO-d6) δ ppm: 13.09 (br s, 1H), 7.89-7.98 (m, 4H), 7.86 (br s, 1H), 6.36 (d, 1H). [ES+MS] m/z 214 (MH+).

WORKUP

后处理

  1. temperatureat reflux for 17 h
  2. customSolvent was evaporated to dryness
  3. customResidue was triturated with EtOH