HRID1054945

反应详情

EQUATION

反应方程式

HRID 1054945 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3,5-dibromo-1-(4-methoxybenzyl)-1H-1,2,4-triazole (1.268 g, 3.65 mmol, Eq: 1.00) and pyrrolidine (273 mg, 317 μl, 3.84 mmol, Eq: 1.05) in dimethyl formamide (12 ml) was heated for 18 hours to 110° C. under argon atmosphere. The crude material was applied on silicagel and purified by flash chromatography over a 50 g silicagel column using heptane/ethyl acetate 30-50% as eluent affording 3-bromo-1-(4-methoxy-benzyl)-5-pyrrolidin-1-yl-1H-[1,2,4]triazole (608 mg/49.3%) as a colorless oil. MS: m/e=338339 (M+H+)

WORKUP

后处理

  1. temperaturewas heated for 18 hours to 110° C. under argon atmosphere
  2. custompurified by flash chromatography over a 50 g silicagel column