1-fluoro-4-[(4-fluorophenyl)methyl]benzene

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The procedure of Example 2 is used except that the 4,4'-difluorodiphenylmethane, water, and sulfuric acid are first mixed, then heated before the MnO2 is added. The yield is 54% 4,4'-difluorobenzophenone that is 95% pure. are first mixed is added

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The procedure of Example 1 was used except that 20 g 4,4'-difluorodiphenylmethane, 30 g water, 31 g MnO2 and 50 g H2 SO4 were used. 20 g off-white solids, after toluene removal, afforded 95% pure 4,4'-difluorobenzophenone in a 90% yield. 20 g off-white solids, after toluene removal

反応条件: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 250 mL round bottomed flask equipped with a heating mantle, overhead agitator, thermometer, condenser, and addition funnel with a tube protruding below the liquid level was added 10.6 g 4,4'-difluorodiphenylmethane (0.051 moles). Agitation was begun and a slurry of 20.5 g MnO2 (0.195 moles) in 30 g water was added to the flask. About 30 g of water were used to wash the MnO2 beaker and were added to the flask. The mixture was allowed to reach about 100° C. at which point 50 g H2SO4 (0.487 moles) were added to the addition funnel. The H2SO4 was then added dropwise into the flask and the reaction temperature slowly rose to about 125° C. when all of the acid had been added. The mixture was heated to maintain the temperature at about 125° C. until gas chromatography showed complete conversion after approximately 12 hours. The reaction mixture was allowed to cool to 100° C. and 50 g toluene were added to the mixture. A slurry of 6 g diatomaceous earth in 30 g water was poured into a vacuum Buchner funnel fitted with No. 42 filter paper to form a filter pre-coat. The contents of the round bottomed flask were then vacuum filtered. 10 g toluene was used to wash the flask and, subsequently, the filter cake. The filter cake was then washed with 100 g toluene heated to about 50° to 70° C. and the filtrate phase separated. The toluene was removed from the organic phase by heating to approximately 65° C. at 10 mm Hg. The 10 g yellow solids assayed as 95% pure 4,4'-difluorobenzophenone for an 84% yield. The solids were recrystallized from a hexane solvent leaving 7.7 g crystalline 4,4'-difluorobenzophenone for a 68% yield. To a 250 mL round bottomed flask equipped with a heating mantle, overhead agitator thermometer, condenser, and addition funnel with a tube protruding below the liquid level to wash the MnO2 beaker were added to the flask to reach about 100° C. at which were added to the addition funnel slowly rose to about 125° C. had been added The mixture was heated after approximately 12 hours to cool to 100° C. fitted with No 42 filter paper to form a filter pre-coat vacuum filtered to wash the flask The filter cake was then washed with 100 g toluene heated to about 50° to 70° C. the filtrate phase separated The toluene was removed from the organic phase by heating to approximately 65° C. at 10 mm Hg The solids were recrystallized from a hexane solvent

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The procedure of Example 2 is used except that the 4,4'-difluorodiphenylmethane, water, and sulfuric acid are first mixed, then heated before the MnO2 is added. The yield is 54% 4,4'-difluorobenzophenone that is 95% pure. are first mixed is added

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The procedure of Example 1 was used except that 20 g 4,4'-difluorodiphenylmethane, 30 g water, 31 g MnO2 and 50 g H2 SO4 were used. 20 g off-white solids, after toluene removal, afforded 95% pure 4,4'-difluorobenzophenone in a 90% yield. 20 g off-white solids, after toluene removal

反応条件: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 250 mL round bottomed flask equipped with a heating mantle, overhead agitator, thermometer, condenser, and addition funnel with a tube protruding below the liquid level was added 10.6 g 4,4'-difluorodiphenylmethane (0.051 moles). Agitation was begun and a slurry of 20.5 g MnO2 (0.195 moles) in 30 g water was added to the flask. About 30 g of water were used to wash the MnO2 beaker and were added to the flask. The mixture was allowed to reach about 100° C. at which point 50 g H2SO4 (0.487 moles) were added to the addition funnel. The H2SO4 was then added dropwise into the flask and the reaction temperature slowly rose to about 125° C. when all of the acid had been added. The mixture was heated to maintain the temperature at about 125° C. until gas chromatography showed complete conversion after approximately 12 hours. The reaction mixture was allowed to cool to 100° C. and 50 g toluene were added to the mixture. A slurry of 6 g diatomaceous earth in 30 g water was poured into a vacuum Buchner funnel fitted with No. 42 filter paper to form a filter pre-coat. The contents of the round bottomed flask were then vacuum filtered. 10 g toluene was used to wash the flask and, subsequently, the filter cake. The filter cake was then washed with 100 g toluene heated to about 50° to 70° C. and the filtrate phase separated. The toluene was removed from the organic phase by heating to approximately 65° C. at 10 mm Hg. The 10 g yellow solids assayed as 95% pure 4,4'-difluorobenzophenone for an 84% yield. The solids were recrystallized from a hexane solvent leaving 7.7 g crystalline 4,4'-difluorobenzophenone for a 68% yield. To a 250 mL round bottomed flask equipped with a heating mantle, overhead agitator thermometer, condenser, and addition funnel with a tube protruding below the liquid level to wash the MnO2 beaker were added to the flask to reach about 100° C. at which were added to the addition funnel slowly rose to about 125° C. had been added The mixture was heated after approximately 12 hours to cool to 100° C. fitted with No 42 filter paper to form a filter pre-coat vacuum filtered to wash the flask The filter cake was then washed with 100 g toluene heated to about 50° to 70° C. the filtrate phase separated The toluene was removed from the organic phase by heating to approximately 65° C. at 10 mm Hg The solids were recrystallized from a hexane solvent

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The procedure of Example 2 is used except that the 4,4'-difluorodiphenylmethane, water, and sulfuric acid are first mixed, then heated before the MnO2 is added. The yield is 54% 4,4'-difluorobenzophenone that is 95% pure. are first mixed is added

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The procedure of Example 1 was used except that 20 g 4,4'-difluorodiphenylmethane, 30 g water, 31 g MnO2 and 50 g H2 SO4 were used. 20 g off-white solids, after toluene removal, afforded 95% pure 4,4'-difluorobenzophenone in a 90% yield. 20 g off-white solids, after toluene removal

反応条件: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a 250 mL round bottomed flask equipped with a heating mantle, overhead agitator, thermometer, condenser, and addition funnel with a tube protruding below the liquid level was added 10.6 g 4,4'-difluorodiphenylmethane (0.051 moles). Agitation was begun and a slurry of 20.5 g MnO2 (0.195 moles) in 30 g water was added to the flask. About 30 g of water were used to wash the MnO2 beaker and were added to the flask. The mixture was allowed to reach about 100° C. at which point 50 g H2SO4 (0.487 moles) were added to the addition funnel. The H2SO4 was then added dropwise into the flask and the reaction temperature slowly rose to about 125° C. when all of the acid had been added. The mixture was heated to maintain the temperature at about 125° C. until gas chromatography showed complete conversion after approximately 12 hours. The reaction mixture was allowed to cool to 100° C. and 50 g toluene were added to the mixture. A slurry of 6 g diatomaceous earth in 30 g water was poured into a vacuum Buchner funnel fitted with No. 42 filter paper to form a filter pre-coat. The contents of the round bottomed flask were then vacuum filtered. 10 g toluene was used to wash the flask and, subsequently, the filter cake. The filter cake was then washed with 100 g toluene heated to about 50° to 70° C. and the filtrate phase separated. The toluene was removed from the organic phase by heating to approximately 65° C. at 10 mm Hg. The 10 g yellow solids assayed as 95% pure 4,4'-difluorobenzophenone for an 84% yield. The solids were recrystallized from a hexane solvent leaving 7.7 g crystalline 4,4'-difluorobenzophenone for a 68% yield. To a 250 mL round bottomed flask equipped with a heating mantle, overhead agitator thermometer, condenser, and addition funnel with a tube protruding below the liquid level to wash the MnO2 beaker were added to the flask to reach about 100° C. at which were added to the addition funnel slowly rose to about 125° C. had been added The mixture was heated after approximately 12 hours to cool to 100° C. fitted with No 42 filter paper to form a filter pre-coat vacuum filtered to wash the flask The filter cake was then washed with 100 g toluene heated to about 50° to 70° C. the filtrate phase separated The toluene was removed from the organic phase by heating to approximately 65° C. at 10 mm Hg The solids were recrystallized from a hexane solvent