HRID2206783

反应详情

EQUATION

反应方程式

HRID 2206783 的结构方程式

PROCEDURE

实验过程

A solution of 1-(allyloxy)-5-bromo-2-chloro-3-(4-methoxybenzyl)benzene (1.20 g, 3.26 mmol) in diethylaniline (3 mL) was heated in a sealed tube at 200° C. for 24 h under nitrogen atmosphere. The mixture was cooled to room temperature and quenched by slow addition of 1 M HCl (50-100 mL). The mixture was extracted with ethyl acetate (100-150 mL). The organic layer was dried over anhydrous MgSO4, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography to provide the compound 216 (1.10 g, 2.99 mmol, 92%).

WORKUP

后处理

  1. customquenched by slow addition of 1 M HCl (50-100 mL)
  2. extractionThe mixture was extracted with ethyl acetate (100-150 mL)
  3. dry with materialThe organic layer was dried over anhydrous MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by silica gel column chromatography