methyl 2,3,4,5-tetrafluorobenzoate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

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: Into a 100 ml glass reactor equipped with a reflux condenser and a stirrer, 20 g (0.091 mol) of the tetrafluorophthalic anhydride prepared in Example 3 and 32.2 g (0.091 mol) of tri-n-octylamine were charged and 3.5 g (0.109 mol) of methanol was dropwise added thereto. Then, the mixture was reacted at 140° C. for 4 hours. After completion of the reaction, the reaction mixture was separated by distillation to obtain 17.5 g of 3,4,5,6-tetrafluorobenzoic acid methyl ester. The yield was 92.3%. Into a 100 ml glass reactor equipped with a reflux condenser and a stirrer Then, the mixture was reacted at 140° C. for 4 hours After completion of the reaction the reaction mixture was separated by distillation

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

実験手順: Into a 100 ml glass reactor equipped with a reflux condenser and a stirrer, 20 g (0.091 mol) of the tetrafluorophthalic anhydride prepared in Example 3 and 32.2 g (0.091 mol) of tri-n-octylamine were charged and 3.5 g (0.109 mol) of methanol was dropwise added thereto. Then, the mixture was reacted at 140° C. for 4 hours. After completion of the reaction, the reaction mixture was separated by distillation to obtain 17.5 g of 3,4,5,6-tetrafluorobenzoic acid methyl ester. The yield was 92.3%. Into a 100 ml glass reactor equipped with a reflux condenser and a stirrer Then, the mixture was reacted at 140° C. for 4 hours After completion of the reaction the reaction mixture was separated by distillation

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

実験手順: Into a 300 ml three necked flask, 20 g (0.096 mol) of the 2,3,4,5-tetrafluorobenzoic acid-methyl ester prepared in Example 15 and 40 g of 70 wt % sulfuric acid were charged, and the mixture was reacted for 10 hours at 140° C. with stirring. Then, 100 ml of water was added to the reaction solution, and the mixture was left to cool. Then, the mixture was extracted with hot toluene. Then, the solvent was distilled off to obtain 17.1 g of 2,3,4,5-tetrafluorobenzoic acid. The yield was 92%. the mixture was reacted for 10 hours at 140° C. the mixture was left to cool Then, the mixture was extracted with hot toluene Then, the solvent was distilled off

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

実験手順: Into a 300 ml three necked flask, 20 g (0.096 mol) of the 2,3,4,5-tetrafluorobenzoic acid-methyl ester prepared in Example 15 and 40 g of 70 wt % sulfuric acid were charged, and the mixture was reacted for 10 hours at 140° C. with stirring. Then, 100 ml of water was added to the reaction solution, and the mixture was left to cool. Then, the mixture was extracted with hot toluene. Then, the solvent was distilled off to obtain 17.1 g of 2,3,4,5-tetrafluorobenzoic acid. The yield was 92%. the mixture was reacted for 10 hours at 140° C. the mixture was left to cool Then, the mixture was extracted with hot toluene Then, the solvent was distilled off

反応条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a 100 ml three necked flask, 20 g (0.079 mol) of the 3,4,5,6-tetrafluorophthalic acid-monomethyl ester prepared in Example 14, and 2.8 g (0.0079 mol) of tri-n-octylamine were charged, and the mixture was heated and stirred at 140° C. for 24 hours. After completion of the reaction, the reaction mixture was separated by distillation to obtain 14.2 g of 2,3,4,5-tetrafluorobenzoic acid methyl ester. The yield was 86.3%. the mixture was heated After completion of the reaction the reaction mixture was separated by distillation

反応条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a 100 ml three necked flask, 20 g (0.079 mol) of the 3,4,5,6-tetrafluorophthalic acid-monomethyl ester prepared in Example 14, and 2.8 g (0.0079 mol) of tri-n-octylamine were charged, and the mixture was heated and stirred at 140° C. for 24 hours. After completion of the reaction, the reaction mixture was separated by distillation to obtain 14.2 g of 2,3,4,5-tetrafluorobenzoic acid methyl ester. The yield was 86.3%. the mixture was heated After completion of the reaction the reaction mixture was separated by distillation

反応条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a 100 ml three necked flask, 20 g (0.079 mol) of the 3,4,5,6-tetrafluorophthalic acid-monomethyl ester prepared in Example 14, and 27.9 g (0.079 mol) of tri-n-octylamine were charged, and the mixture was heated and stirred at 140° C. for 4 hours. After completion of the reaction, the reaction mixture was separated by distillation to obtain 15.5 g of 2,3,4,5-tetrafluorobenzoic acid methyl ester. The yield was 94.2%. the mixture was heated After completion of the reaction the reaction mixture was separated by distillation

反応条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Into a 100 ml three necked flask, 20 g (0.079 mol) of the 3,4,5,6-tetrafluorophthalic acid-monomethyl ester prepared in Example 14, and 27.9 g (0.079 mol) of tri-n-octylamine were charged, and the mixture was heated and stirred at 140° C. for 4 hours. After completion of the reaction, the reaction mixture was separated by distillation to obtain 15.5 g of 2,3,4,5-tetrafluorobenzoic acid methyl ester. The yield was 94.2%. the mixture was heated After completion of the reaction the reaction mixture was separated by distillation

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

実験手順: Into a 100 ml glass reactor equipped with a reflux condenser and a stirrer, 20 g (0.091 mol) of the tetrafluorophthalic anhydride prepared in Example 3 and 32.2 g (0.091 mol) of tri-n-octylamine were charged and 3.5 g (0.109 mol) of methanol was dropwise added thereto. Then, the mixture was reacted at 140° C. for 4 hours. After completion of the reaction, the reaction mixture was separated by distillation to obtain 17.5 g of 3,4,5,6-tetrafluorobenzoic acid methyl ester. The yield was 92.3%. Into a 100 ml glass reactor equipped with a reflux condenser and a stirrer Then, the mixture was reacted at 140° C. for 4 hours After completion of the reaction the reaction mixture was separated by distillation