反应详情

温度

2.5 °C

4-Amino-2,6-dichlorobenzoic acid methyl ester (1.00 g) was suspended in 40% aq. HBr and the mixture was cooled lto 0-5° C. After NaNO2 (376 mg) was added in small portions, the mixture was stirred for about 5 min. Copper (100 mg) was added and the mixture was warmed up to 100° C. The mixture was then stirred at 100° C. for 30 min, diluted with water and extracted with AcOEt. The extract was dried (MgSO4), filtered and evaporated. The residue was purified by column chromatography (silica gel; eluent: hexane and AcOEt 50:1) to give 4-bromo-2,6-dichlorobenzoic acid methyl ester (1.07 g).

1. temperaturethe mixture was warmed up to 100° C
2. stirringThe mixture was then stirred at 100° C. for 30 min
3. extractionextracted with AcOEt
4. dry with materialThe extract was dried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by column chromatography (silica gel; eluent: hexane and AcOEt 50:1)