HRID880490
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was heated
- temperatureto reflux for 9 h
- filtrationfiltered
- washthe residue was washed with carbon tetrachloride
- washThe combined filtrates were washed with water, sodium bicarbonate solution, brine
- dry with materialdried over anhydrous sodium sulphate
- concentrationconcentrated in vacuo
- customThe crude product was purified over silica gel (60-120 mesh) with 30% ethyl acetate/hexane as eluent