反应详情

温度

60 °C

A mixture of AlCl3 (1040 g, 7878.7 mmol) in 1-bromo-2,4-difluorobenzene ([CAS 348-57-2], 600 g, 3108.9 mmol) was stirred for 10 min at 60° C. Acetyl chloride [CAS 75-36-5], 366 g, 4662.4 mmol) was added dropwise in the reaction mixture for 4 h at 60° C. The mixture was stirred an additional 6 h at 95° C. The reaction mixture was cooled to −10° C. Ice (2450 g) was added for 1.5 h. HCl (12 N, 1500 mL) was added and the mixture was stirred for 1 h. EtOAc (9000 mL) was added and the organic layer was washed with water, dried over Na2SO4 and filtered. After concentration, the residue was purified by column chromatography over silica gel (eluent: petroleum ether/EtOAc, 50/1) to yield I-18 (300 g, 41%).

1. stirringThe mixture was stirred an additional 6 h at 95° C
2. temperatureThe reaction mixture was cooled to −10° C
3. stirringthe mixture was stirred for 1 h
4. washthe organic layer was washed with water
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationAfter concentration
8. customthe residue was purified by column chromatography over silica gel (eluent: petroleum ether/EtOAc, 50/1)
9. customto yield I-18 (300 g, 41%)