2-(2,3-difluorophenyl)-2-methylpropanenitrile

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

実験手順: Hydrolysis of 2-(2,3-difluorophenyl)-2-methylpropionitrile was performed according to the procedure of Example 10 using sodium hydroxide in the presence of hydrogen peroxide to provide 2-(2,3-difluorophenyl)isobutyramide [1H-NMR (CDCl3): δ 7.17-7.08 (m, 3H), 5.98 (br s, 1H), 5.45 (br s, 1H), 1.60 (s, 6H)].

反応条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2-(2,3-difluorophenyl)-2-methylpropanenitrile (9.5 g, 52 mmol) in 50 mL dioxane was treated with 10 mL H2O and concentrated H2SO4 (3 mL, 105 mmol). The resulting mixture was stirred at 110° C. for 16 hours, M+1=201. The reaction was then cooled to room temperature. The mixture was extracted with EtOAc and the organic layer discarded. The water layer was acidified with concentrated HCl, extracted with EtOAc, washed with H2O and brine, dried over anhydrous Na2SO4, and concentrated in vacuo to give 4.74 g of the title compound as a pale yellow solid. MS (m/z)=201 (M+H)+. The reaction was then cooled to room temperature The mixture was extracted with EtOAc extracted with EtOAc washed with H2O and brine dried over anhydrous Na2SO4 concentrated in vacuo

反応条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 2-(2,3-difluorophenyl)-2-methylpropanenitrile (9.5 g, 52 mmol) in 50 mL dioxane was treated with 10 mL H2O and concentrated H2SO4 (3 mL, 105 mmol). The resulting mixture was stirred at 110° C. for 16 hours, M+1=201. The reaction was then cooled to room temperature. The mixture was extracted with EtOAc and the organic layer discarded. The water layer was acidified with concentrated HCl, extracted with EtOAc, washed with H2O and brine, dried over anhydrous Na2SO4, and concentrated in vacuo to give 4.74 g of the title compound as a pale yellow solid. MS (m/z)=201 (M+H)+. The reaction was then cooled to room temperature The mixture was extracted with EtOAc extracted with EtOAc washed with H2O and brine dried over anhydrous Na2SO4 concentrated in vacuo

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

実験手順: Hydrolysis of 2-(2,3-difluorophenyl)-2-methylpropionitrile was performed according to the procedure of Example 10 using sodium hydroxide in the presence of hydrogen peroxide to provide 2-(2,3-difluorophenyl)isobutyramide [1H-NMR (CDCl3): δ 7.17-7.08 (m, 3H), 5.98 (br s, 1H), 5.45 (br s, 1H), 1.60 (s, 6H)].