methyl 2-(cyanomethyl)-3-fluorobenzoate

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

実験手順: Ethanol and Raney nickel (Aldrich) were added to 2-cyanomethyl-3-fluoro-benzoic acid methyl ester (3.3 g, 17 mmol) to carry out catalytic reduction under ordinary pressure at 50° C. for 7 hours and then at room temperature for 15 hours. Raney nickel was removed from the reaction solution by filtration, the solvent was removed by evaporation under a reduced pressure, and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 2.1 g (13 mmol, 74% in yield) of the title compound. at 50° C. for 7 hours Raney nickel was removed from the reaction solution by filtration the solvent was removed by evaporation under a reduced pressure the thus obtained material was separated purified by a silica gel column chromatography to obtain

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-Bromomethyl-3-fluoro-benzoic acid methyl ester (5.1 g, 21 mmol) was dissolved in methanol (50 ml), and sodium cyanide aqueous solution (4.2 ml, 5 ml, 21 mmol) was added dropwise thereto. After completion of the dropwise addition, the mixture was stirred at 50° C. for 2 hours. The residue obtained by evaporating the solvent from the reaction solution under a reduced pressure was mixed with ethyl acetate, washed with water and saturated brine and then dried with anhydrous it magnesium sulfate. The solvent was removed by evaporation from the organic layer under a reduced pressure, and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 3.3 g (17 mmol, 82% in yield) of the title compound. After completion of the dropwise addition The residue obtained by evaporating the solvent from the reaction solution under a reduced pressure was mixed with ethyl acetate washed with water and saturated brine dried with anhydrous it magnesium sulfate The solvent was removed by evaporation from the organic layer under a reduced pressure the thus obtained material was separated purified by a silica gel column chromatography to obtain

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-Bromomethyl-3-fluoro-benzoic acid methyl ester (5.1 g, 21 mmol) was dissolved in methanol (50 ml), and sodium cyanide aqueous solution (4.2 ml, 5 ml, 21 mmol) was added dropwise thereto. After completion of the dropwise addition, the mixture was stirred at 50° C. for 2 hours. The residue obtained by evaporating the solvent from the reaction solution under a reduced pressure was mixed with ethyl acetate, washed with water and saturated brine and then dried with anhydrous it magnesium sulfate. The solvent was removed by evaporation from the organic layer under a reduced pressure, and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 3.3 g (17 mmol, 82% in yield) of the title compound. After completion of the dropwise addition The residue obtained by evaporating the solvent from the reaction solution under a reduced pressure was mixed with ethyl acetate washed with water and saturated brine dried with anhydrous it magnesium sulfate The solvent was removed by evaporation from the organic layer under a reduced pressure the thus obtained material was separated purified by a silica gel column chromatography to obtain

反応条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-Bromomethyl-3-fluoro-benzoic acid methyl ester (5.1 g, 21 mmol) was dissolved in methanol (50 ml), and sodium cyanide aqueous solution (4.2 ml, 5 ml, 21 mmol) was added dropwise thereto. After completion of the dropwise addition, the mixture was stirred at 50° C. for 2 hours. The residue obtained by evaporating the solvent from the reaction solution under a reduced pressure was mixed with ethyl acetate, washed with water and saturated brine and then dried with anhydrous it magnesium sulfate. The solvent was removed by evaporation from the organic layer under a reduced pressure, and the thus obtained material was separated and purified by a silica gel column chromatography to obtain 3.3 g (17 mmol, 82% in yield) of the title compound. After completion of the dropwise addition The residue obtained by evaporating the solvent from the reaction solution under a reduced pressure was mixed with ethyl acetate washed with water and saturated brine dried with anhydrous it magnesium sulfate The solvent was removed by evaporation from the organic layer under a reduced pressure the thus obtained material was separated purified by a silica gel column chromatography to obtain