反应详情

温度

-60 °C

A total of 716 mg of aluminium chloride was suspended in 24.4 ml of dichloromethane and was then mixed with 0.65 ml of 3-fluorobenzoyl chloride and 1 g of 1-bromo-4-fluoro-2-methoxy-benzene obtained in Production Example II-1-a under stirring at −60° C. The mixture was raised in temperature to room temperature over 2.5 hours and was stirred for further 3 hours. Water was added to the reaction mixture under ice-cooling, followed by extracting with diethyl ether. The resulting organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and brine, dried over magnesium sulfate and the solvent was evaporated. The residue was purified and separated by silica gel column chromatography (ethyl acetate:hexane=1:10), to give 856 mg of the title compound as white crystals.

1. temperatureThe mixture was raised in temperature to room temperature over 2.5 hours
2. stirringwas stirred for further 3 hours
3. temperaturecooling
4. extractionby extracting with diethyl ether
5. washThe resulting organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and brine
6. dry with materialdried over magnesium sulfate
7. customthe solvent was evaporated
8. customThe residue was purified
9. customseparated by silica gel column chromatography (ethyl acetate:hexane=1:10)