HRID880490

反应详情

EQUATION

反应方程式

HRID 880490 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 5-methyl-2-(4-nitrophenyl)oxazole (3.2 g, 15.68 mmol) and benzoyl peroxide (10 mg, catalytic) in carbon tetrachloride (20 mL), was added N-bromo succinamide (2.77 g, 15.68 mmol). The mixture was heated to reflux for 9 h, filtered and the residue was washed with carbon tetrachloride. The combined filtrates were washed with water, sodium bicarbonate solution, brine, dried over anhydrous sodium sulphate and concentrated in vacuo. The crude product was purified over silica gel (60-120 mesh) with 30% ethyl acetate/hexane as eluent to afford 5-(bromomethyl)-2-(4-nitro-phenyl)-oxazole (2.9 g, 65%) as a solid.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 9 h
  3. filtrationfiltered
  4. washthe residue was washed with carbon tetrachloride
  5. washThe combined filtrates were washed with water, sodium bicarbonate solution, brine
  6. dry with materialdried over anhydrous sodium sulphate
  7. concentrationconcentrated in vacuo
  8. customThe crude product was purified over silica gel (60-120 mesh) with 30% ethyl acetate/hexane as eluent