4'-(溴甲基)-2-氟-1,1'-联苯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 8.70 g of 2-fluoro-4′-methylbiphenyl, 8.32 g of N-bromosuccinimide, 0.10 g of 2,2′-azobisisobutylonitrile and 150 ml of carbon tetrachloride was heat-refluxed for 5 hours. The reaction solution was washed with water, and the organic layer was concentrated. The resulting residue was purified through silica-gel column chromatography (eluent: a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4′-bromomethylbiphenyl. Further, this compound was crystallized from hexane to give 4.93 g of 2-fluoro-4′-bromomethylbiphenyl. was heat-refluxed for 5 hours The reaction solution was washed with water the organic layer was concentrated The resulting residue was purified through silica-gel column chromatography (eluent a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4′-bromomethylbiphenyl Further, this compound was crystallized from hexane

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 8.70 g of 2-fluoro-4′-methylbiphenyl, 8.32 g of N-bromosuccinimide, 0.10 g of 2,2′-azobisisobutylonitrile and 150 ml of carbon tetrachloride was heat-refluxed for 5 hours. The reaction solution was washed with water, and the organic layer was concentrated. The resulting residue was purified through silica-gel column chromatography (eluent: a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4′-bromomethylbiphenyl. Further, this compound was crystallized from hexane to give 4.93 g of 2-fluoro-4′-bromomethylbiphenyl. was heat-refluxed for 5 hours The reaction solution was washed with water the organic layer was concentrated The resulting residue was purified through silica-gel column chromatography (eluent a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4′-bromomethylbiphenyl Further, this compound was crystallized from hexane

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 8.70 g of 2-fluoro-4′-methylbiphenyl, 8.32 g of N-bromosuccinimide, 0.10 g of 2,2′-azobisisobutylonitrile and 150 ml of carbon tetrachloride was heat-refluxed for 5 hours. The reaction solution was washed with water, and the organic layer was concentrated. The resulting residue was purified through silica-gel column chromatography (eluent: a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4′-bromomethylbiphenyl. Further, this compound was crystallized from hexane to give 4.93 g of 2-fluoro-4′-bromomethylbiphenyl. was heat-refluxed for 5 hours The reaction solution was washed with water the organic layer was concentrated The resulting residue was purified through silica-gel column chromatography (eluent a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4′-bromomethylbiphenyl Further, this compound was crystallized from hexane

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 2-fluoro-4′-methylbiphenyl (8.70 g), N-bromosuccinimide (8.32 g), 2,2′-azobisisobutyronitrile (0.10 g) and carbon tetrachloride (150 ml) is refluxed by heating for five hours. The reaction solution is washed with water. The residue, which is obtained by concentrating the organic layer, is purified using silica gel column chromatography (eluate: hexane/ethyl acetate=9/1) and thus, preliminarily purified 2-fluoro-4′-bromomethylbiphenyl is obtained. Furthermore, crystallization using hexane produced 2-fluoro-4′-bromomethylbiphenyl (4.93 g). 1H-NMR (CDCl3, δ): 4.55 (2H, s), 7.13-7.23 (2H, m), 7.33 (1H, m), 7.43 (1H, m), 7.47 (2H, d, J=8.1 Hz), 7.54 (2H, d, J=8.1 Hz). is refluxed by heating for five hours The reaction solution is washed with water The residue, which is obtained by concentrating the organic layer is purified

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 8.70 g of 2-fluoro-4'-methylbiphenyl, 8.32 g of N-bromosuccinimide, 0.10 g of 2,2'-azobisisobutylonitrile and 150 ml of carbon tetrachloride was heat-refluxed for 5 hours. The reaction solution was washed with water, and the organic layer was concentrated. The resulting residue was purified through silica-gel column chromatography (eluent: a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4'-bromomethylbiphenyl. Further, this compound was crystallized from hexane to give 4.93 g of 2-fluoro-4'-bromomethylbiphenyl. was heat-refluxed for 5 hours The reaction solution was washed with water the organic layer was concentrated The resulting residue was purified through silica-gel column chromatography (eluent a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4'-bromomethylbiphenyl Further, this compound was crystallized from hexane

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 8.70 g of 2-fluoro-4′-methylbiphenyl, 8.32 g of N-bromosuccinimide, 0.10 g of 2,2′-azobisisobutylonitrile and 150 ml of carbon tetrachloride was heat-refluxed for 5 hours. The reaction solution was washed with water, and the organic layer was concentrated. The resulting residue was purified through silica-gel column chromatography (eluent: a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4′-bromomethylbiphenyl. Further, this compound was crystallized from hexane to give 4.93 g of 2-fluoro-4′-bromomethylbiphenyl. was heat-refluxed for 5 hours The reaction solution was washed with water the organic layer was concentrated The resulting residue was purified through silica-gel column chromatography (eluent a mixture of hexane and ethyl acetate at a ratio of 9:1) to obtain crude 2-fluoro-4′-bromomethylbiphenyl Further, this compound was crystallized from hexane