HRID403502

反应详情

EQUATION

反应方程式

HRID 403502 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a 500 ml, four-necked flask equipped with an overhead stirrer, a thermocouple and a condenser was charged with 4-((5-amino-3-ethyl-1H-pyrazol-4-yl)methyl)benzonitrile (26) (12.8 g, 56.5 mmol), pentane-2,4-dione (6.8 g, 67.9 mmol, 1.2 eq), 20 ml of HOAc and 40 ml of concentrated HCl. The mixture was stirred at 110° C. for 43 hours. It was cooled to room temperature and 300 ml of water was added. Slowly, the solution became a suspension. It was stirred at room temperature for 1 h. The precipitate was collected by vacuum filtration and the solid was washed with water. The solid was vacuum oven dried at 50° C. for 5 h.

WORKUP

后处理

  1. customTo a 500 ml, four-necked flask equipped with an overhead stirrer
  2. temperatureIt was cooled to room temperature
  3. stirringIt was stirred at room temperature for 1 h
  4. filtrationThe precipitate was collected by vacuum filtration
  5. washthe solid was washed with water
  6. customdried at 50° C. for 5 h.