HRID2232225

反应详情

EQUATION

反应方程式

HRID 2232225 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

50% Sodium hydride in mineral oil (1 g) is suspended in anhydrous dimethylformamide (50 ml) and stirred for 10 minutes. Then a solution of ethanethiol (1.5 ml) in anhydrous dimethylformamide (10 ml) is slowly added thereto and the resulting mixture is stirred at room temperature for 30 minutes. Finally 6-chloro-3-phenyl-1,2,4-triazolo[3,4-a]phthalazine (5.9 g) is added and the reaction mixture is heated at 50° C. for five hours. The solvent is evaporated off under vacuum and the obtained residue is washed a few times with water and then is crystallized from isopropanol yielding 4.7 g of the compound of the title. M.p. 190°-91° C.

WORKUP

后处理

  1. stirringthe resulting mixture is stirred at room temperature for 30 minutes
  2. customThe solvent is evaporated off under vacuum
  3. washthe obtained residue is washed a few times with water
  4. customis crystallized from isopropanol yielding 4.7 g of the compound of the title