HRID444822

反应详情

EQUATION

反应方程式

HRID 444822 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.34 g (32.3 mmol) of N-[1-(5-oxo-3-phenyl-4,5-dihydro-1,2,4-triazin-6-yl)ethyl]acetamide] (Example 14A) were dissolved in 330 ml of 1,2-dichloroethane and 4.5 ml (48.5 mmol) of phosphoryl chloride were added. The mixture was stirred under reflux for 24 h. After cooling, the precipitate was filtered off and washed with water and diethyl ether. The product was subsequently dried under high vacuum. This gave 4.6 g (59% of theory) of the product as a solid.

WORKUP

后处理

  1. temperatureunder reflux for 24 h
  2. temperatureAfter cooling
  3. filtrationthe precipitate was filtered off
  4. washwashed with water and diethyl ether
  5. customThe product was subsequently dried under high vacuum