反应详情

Methyl 4-methyl-3-chlorobenzoate (4.5 g, 0.024 mol) was dissolved in carbon tetrachloride (100 ml), and thereto were added N-bromosuccinimide (4.8 g, 0.026 mol) and a catalytic amount of perbenzoic anhydride. The mixture was heated and refluxed under nitrogen atmosphere for 2 hours, allowed to cool, and the precipitate was separated by filtration. The filtrate was concentrated, and separated and purified by using a silica-gel column chromatography (ethyl acetate:n-hexane=1:20) to give the title compound (4.7 g, 0.018 mol) (yield 75%).

1. temperatureThe mixture was heated
2. temperaturerefluxed under nitrogen atmosphere for 2 hours
3. temperatureto cool
4. customthe precipitate was separated by filtration
5. concentrationThe filtrate was concentrated
6. customseparated
7. custompurified