反应详情

To a solution of 3-methylphenylacetic acid (125 g) in tetrachloro methane (1660 ml), N-bromosuccinimide (148 g) and 2,2′-azobisisobutyronitrile (AIBN; 1.37 g) were added. The mixture was refluxed with heating. After termination of reaction, the solution was cooled with ice. The white precipitate was filtered by glass-filter. The filtrate was washed by tetrachloro methane. The filtrate together with washing liquid was concentrated. The obtained residue was dissolved into ethyl acetate. Thereto, hexane was added. The mixture was crystallized to obtain the title compound (59 g).

1. temperatureThe mixture was refluxed
2. temperaturewith heating
3. customAfter termination of reaction
4. temperaturethe solution was cooled with ice
5. filtrationThe white precipitate was filtered
6. filtrationby glass-filter
7. washThe filtrate was washed by tetrachloro methane
8. washThe filtrate together with washing liquid
9. concentrationwas concentrated
10. dissolutionThe obtained residue was dissolved into ethyl acetate
11. additionThereto, hexane was added
12. customThe mixture was crystallized