HRID1013040

反应详情

EQUATION

反应方程式

HRID 1013040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a suspension of 2-bromobenzyl bromide (500 mg, 2.00 mmol) and 4-methoxyphenylhydrazine hydrochloride (348 mg, 2.00 mmol) in N,N-dimethylformamide (8 mL) was added potassium carbonate (1.38 g, 10.0 mmol). The reaction mixture was heated at 90° C. for 4 hours. The reaction was partitioned between water and methylene chloride. The methylene chloride was dried (MgSO4), concentrated and purified by SiO2 chromatography with 10-50% ethyl acetate/hexanes to give 298 mg of the title compound. LC-MS (C14H18BrN2O calculated 306) m/z 307 (M+H).

WORKUP

后处理

  1. customThe reaction was partitioned between water and methylene chloride
  2. dry with materialThe methylene chloride was dried (MgSO4)
  3. concentrationconcentrated
  4. custompurified by SiO2 chromatography with 10-50% ethyl acetate/hexanes