HRID271421

反应详情

EQUATION

反应方程式

HRID 271421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 7-(4-chlorophenyl)-5-(methylthio)-8-phenyl-[1,2,4]triazolo[4,3-c]pyrimidin-3(2H)-one (100 mg, 0.27 mmol) in DMF (2 mL) at room temperature under argon was added 4-trifluoromethylbenzyl bromide (77.7 mg, 0.33 mmol), followed by K2CO3 (74.5 mg, 0.54 mmol). The resulting mixture was stirred at room temperature for 5 h. Insoluble material was filtered off and the filtrate was purified by silica gel column chromatography eluted with ethyl acetate-hexanes, then lyophilized from 1,4-dioxane, to obtain the title compound (112 mg) as an off-white lyophilate. HPLC/MS: retention time=4.50 min, [M+H]30 =527.

WORKUP

后处理

  1. filtrationInsoluble material was filtered off
  2. customthe filtrate was purified by silica gel column chromatography
  3. washeluted with ethyl acetate-hexanes