HRID1475222

反应详情

EQUATION

反应方程式

HRID 1475222 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

To a solution of 5-methyl-1H-1,2,4-triazole-3-carboxamide (2.5 g, 19.8 mmol) and 1-bromo-3-(bromomethyl)benzene (5.45 g, 21.8 mmol) in THF (99 mL), K2CO3 (5.5 g, 39.6 mmol) was added. The mixture was stirred at 50° C. for 18 h, and then the reaction was filtered under vacuum. The solvent was removed under reduced pressure and the crude product was purified on a Biotage pre-packed silica gel column with a gradient of 0% to 20% MeOH:DCM to afford 1-(3-bromobenzyl)-5-methyl-1H-1,2,4-triazole-3-carboxamide (1.5 g, 26%) as a viscous oil. MS (ES+) C11H11BrN4O requires: 294, 296. found: 295, 297 [MH]+(1:1).

WORKUP

后处理

  1. filtrationthe reaction was filtered under vacuum
  2. customThe solvent was removed under reduced pressure
  3. customthe crude product was purified on a Biotage pre-packed silica gel column with a gradient of 0% to 20% MeOH