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4-bromo-2,3-difluoro(bromodifluoromethyl)benzene[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
Under nitrogen atmosphere, diisopropylamine (5.8 g) was dissolved in THF (30 mL) and cooled to -70 ° C. or lower. To the solution, a 1.6 M butyllithium / hexane solution (32 mL) was added dropwise at such a rate that the inner temperature did not reach -65 ° C., and the mixture was subsequently stirred at -70 ° C. or lower for 30 minutes.Subsequently, a solution prepared by dissolving <strong>[38573-88-5]2,3-difluorobromobenzene</strong> (10 g) in THF (50 mL) was added dropwise to the stirring reaction solution at a rate such that the internal temperature did not exceed -65 ° C.,The mixture was stirred at -70 ° C. or lower for 1 hour to prepare phenyllithiums.In a separate reaction vessel, a solution of difluorodibromomethane (16.3 g) dissolved in THF (160 mL) was cooled to -70 ° C. or lower, and a solution of the phenyllithium prepared in advance was added to the solution in a cannula , Followed by stirring at -70 ° C. or lower for 1 hour,And the mixture was heated to room temperature.Water and hexane were added to the reaction solution to separate the organic layer, and the organic layer was washed twice with saturated brine.Sodium sulfate was added to the organic layer after washing, dried, the solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography to obtain 4-bromo-2,3-difluoro- (bromodifluoromethyl) benzene and 1,4 - di<strong>[38573-88-5]bromo-2,3-difluorobenzene</strong> (14.5 g). By measuring the ratio of each compound in the mixture using gas chromatography, 78.5percent of 4-bromo-2,3-difluoro- (bromodifluoromethyl) benzene, 1,4-dibromo- 3-Difluorobenzene was 21.5percent.
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