3468-99-3

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

実験手順: To a solution of diphenylacetic acid (20 g, 0.094 mol) in EtOH (70 mL), was added toluene (70 mL). Next, H2SO4 (3 mL) was added dropwise and the reaction mixture was refluxed for 18 h. Then, H2O and EtOAc were added, the layers were separated, and the organic phase was washed with saturated NaHCO3 solution (3×), dried and concentrated to a white solid (23.2 g), which was directly used in the next step as obtained. the reaction mixture was refluxed for 18 h the layers were separated the organic phase was washed with saturated NaHCO3 solution (3×) dried concentrated to a white solid (23.2 g), which as obtained

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

実験手順: To a solution of diphenylacetic acid (20 g, 0.094 mol) in EtOH (70 mL), was added toluene (70 mL). Next, H2SO4 (3 mL) was added dropwise and the reaction mixture was refluxed for 18 h. Then, H2O and EtOAc were added, the layers were separated, and the organic phase was washed with saturated NaHCO3 solution (3×), dried and concentrated to a white solid (23.2 g), which was directly used in the next step as obtained. the reaction mixture was refluxed for 18 h the layers were separated the organic phase was washed with saturated NaHCO3 solution (3×) dried concentrated to a white solid (23.2 g), which as obtained

反応条件: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The product of Example 1A (5.58 g) was dissolved in anhydrous dioxane (15 mL). Sodium ethoxide (1.58 g) was added, and the mixture was heated to 40-50° C. for 30 minutes. Acrylonitrile (1.44 mL) was added dropwise with stirring. The mixture was heated at 60-70° C. for one hour. The dioxane was removed in vacuo, and the residue was taken up in diethyl ether, washed with water and brine, dried with magnesium sulfate, filtered, and concentrated. The crude material was purified by silica gel chromatography (3-10% ethyl acetate/hexane) to obtain the title compound. MS (DCI+) m/z 311 (M+NH4)+. The mixture was heated at 60-70° C. for one hour The dioxane was removed in vacuo washed with water and brine dried with magnesium sulfate filtered concentrated The crude material was purified by silica gel chromatography (3-10% ethyl acetate/hexane)

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

実験手順: 2,2-Diphenylacetic acid (50 g) was dissolved in ethanol (350 mL). Concentrated sulfuric acid (3 mL) was added, and the mixture was refluxed overnight. After cooling to room temperature, the reaction mixture was concentrated and diluted with diethyl ether. The organic solvent solution was then extracted with water, saturated aqueous sodium bicarbonate solution, and brine. The organic layer was then dried with magnesium sulfate, filtered, and concentrated to obtain the title compound. MS (DCI+) m/z 241 (M+H)+. the mixture was refluxed overnight the reaction mixture was concentrated diluted with diethyl ether The organic solvent solution was then extracted with water, saturated aqueous sodium bicarbonate solution, and brine The organic layer was then dried with magnesium sulfate filtered concentrated

反応条件: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: The product of Example 68A (5.58 g) was dissolved in anhydrous dioxane (15 mL). Sodium ethoxide (1.58 g) was added and the mixture was heated to 40-50° C. for 30 minutes. Acrylonitrile (1.44 mL) was added dropwise with stirring. The mixture was heated at 60-70° C. for one hour. The dioxane was removed in vacuo, and the residue was taken up in diethyl ether, washed with water and brine, dried with magnesium sulfate, filtered, and concentrated. The crude material was purified by silica gel chromatography (3-10% ethyl acetate/hexane) to obtain the title compound. MS (DCI+) m/z 311 (M+NH4)+. The mixture was heated at 60-70° C. for one hour The dioxane was removed in vacuo washed with water and brine dried with magnesium sulfate filtered concentrated The crude material was purified by silica gel chromatography (3-10% ethyl acetate/hexane)

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

実験手順: 2,2-Diphenylacetic acid (50 g) was dissolved in ethanol (350 mL). Concentrated sulfuric acid (3 mL) was added, and the mixture was refluxed overnight. After cooling to room temperature, the reaction mixture was concentrated and diluted with diethyl ether. The organic solvent solution was then extracted with water, saturated aqueous sodium bicarbonate solution, and brine. The organic layer was then dried with magnesium sulfate, filtered, and concentrated to obtain the title compound. MS (DCI+) m/z 241 (M+H)+. the mixture was refluxed overnight the reaction mixture was concentrated diluted with diethyl ether The organic solvent solution was then extracted with water, saturated aqueous sodium bicarbonate solution, and brine The organic layer was then dried with magnesium sulfate filtered concentrated

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

実験手順: To a solution of diphenylacetic acid (20 g, 0.094 mol) in EtOH (70 mL), was added toluene (70 mL). Next, H2SO4 (3 mL) was added dropwise and the reaction mixture was refluxed for 18 h. Then, H2O and EtOAc were added, the layers were separated, and the organic phase was washed with saturated NaHCO3 solution (3×), dried and concentrated to a white solid (23.2 g), which was directly used in the next step as obtained. the reaction mixture was refluxed for 18 h the layers were separated the organic phase was washed with saturated NaHCO3 solution (3×) dried concentrated to a white solid (23.2 g), which as obtained