HRID2183547

反应详情

EQUATION

反应方程式

HRID 2183547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl acetoacetate (0.7 ml) was added to a solution of 4-(2,4,6-Trimethyl-phenyl)-2H-pyrazol-3-ylamine (1.120 g, 5.57 mmol) in 5 ml of acetic acid and the resulting mixture was heated at reflux for two days. Reaction mixture cooled and a white solid formed. Ethanol (6 ml) was added and stirred at room temperature overnight, filtered to give white solid which was recrystallized from ethanol to give 673 mg(45.2%) of the title compound as white crystals. 1H NMR (DMSO-d6) ä 11.9(s, 1H), 7.7(s, 1H), 6.95(s, 2H), 5.55(s, 1H), 2.25(s, 3H), 2.20(s, 3H), 2.0(s, 6H)ppm.

WORKUP

后处理

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for two days
  3. customReaction mixture
  4. temperaturecooled
  5. customa white solid formed
  6. filtrationfiltered
  7. customto give white solid which
  8. customwas recrystallized from ethanol