HRID273743
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
N-Bromosuccinimide (2.35 g) and azo(bisisobutyronitrile) (60 mg) were added to a solution of compound C (3.2 g) in carbon tetrachloride (60 ml). The mixture was heated under reflux for 4 hours and then cooled to ambient temperature. Insoluble material was removed by filtration and the filtrate was concentrated. The residue was recrystallised from hexane to give methyl 2-(5-bromomethyl-benzoxazol-2-yl)benzoate (D) (2.1 g), m.p. 92°-95° C; NMR: 3.9(s, 3H), 4.65(s, 2H), 7.45(dd, 1H), 7.55(dd, 1H), 7.6-7.7(m, 2H), 7.8-7.85(m, 2H), 8.0-8.1(m, 1H).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureunder reflux for 4 hours
- customInsoluble material was removed by filtration
- concentrationthe filtrate was concentrated
- customThe residue was recrystallised from hexane