HRID38674

反应详情

EQUATION

反应方程式

HRID 38674 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 hours. The reaction was allowed to reach room temperature and solvent was evaporated to dryness. Residue was washed with EtOH and a yellowish solid was filtered to afford 23.6 g (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 hours
  2. customto reach room temperature
  3. customsolvent was evaporated to dryness
  4. washResidue was washed with EtOH
  5. filtrationa yellowish solid was filtered