2-(甲基氨基)苯甲腈

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Fluorobenzonitrile (10.0 g, 82.8 mmol) was dissolved in acetonitrile (100 ml), and 40% aqueous methylamine solution (200 ml) was added thereto, followed by stirring at 60° C. overnight. 40% aqueous methylamine solution (100 ml) was further added thereto, followed by stirring at 60° C. for 9 hours. The reaction mixture was concentrated under reduced pressure, then water was added to the resulting residue, the mixture was extracted with chloroform. After the organic layer was dried (over anhydrous magnesium sulfate), the drying agent was filtered off, and the organic layer was concentrated under reduced pressure. The resulting oily substances were purified by silica gel column chromatography (the substances were eluted with an increasing concentration of chloroform from chloroform/hexane=1/2 to chloroform/hexane=1/1) to give the title compound (5.38 g, 49%). by stirring at 60° C. for 9 hours The reaction mixture was concentrated under reduced pressure water was added to the resulting residue the mixture was extracted with chloroform After the organic layer was dried (over anhydrous magnesium sulfate) the drying agent was filtered off the organic layer was concentrated under reduced pressure The resulting oily substances were purified by silica gel column chromatography (the substances were eluted with an increasing concentration of chloroform from chloroform/hexane=1/2 to chloroform/hexane=1/1)

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Fluorobenzonitrile (10.0 g, 82.8 mmol) was dissolved in acetonitrile (100 ml), and 40% aqueous methylamine solution (200 ml) was added thereto, followed by stirring at 60° C. overnight. 40% aqueous methylamine solution (100 ml) was further added thereto, followed by stirring at 60° C. for 9 hours. The reaction mixture was concentrated under reduced pressure, then water was added to the resulting residue, the mixture was extracted with chloroform. After the organic layer was dried (over anhydrous magnesium sulfate), the drying agent was filtered off, and the organic layer was concentrated under reduced pressure. The resulting oily substances were purified by silica gel column chromatography (the substances were eluted with an increasing concentration of chloroform from chloroform/hexane=1/2 to chloroform/hexane=1/1) to give the title compound (5.38 g, 49%). by stirring at 60° C. for 9 hours The reaction mixture was concentrated under reduced pressure water was added to the resulting residue the mixture was extracted with chloroform After the organic layer was dried (over anhydrous magnesium sulfate) the drying agent was filtered off the organic layer was concentrated under reduced pressure The resulting oily substances were purified by silica gel column chromatography (the substances were eluted with an increasing concentration of chloroform from chloroform/hexane=1/2 to chloroform/hexane=1/1)

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: N-(2-Cyanophenyl)-2,2,2-trifluoro-N-methylacetamide (3 g, 0.01 mol) was dissolved in a sodium bicarbonate/water/ethanol mixture, refluxed for 5 h and evaporated. Water was added and the mixture extracted with ethyl acetate, dried over sodium sulphate and evaporated to give the product (2.5 g). MS (+EI) 132 (M+), 1H NMR (CDCl3) 7.45 (2H, t), 6.69 (1H, d), 6.62 (1H, t), 6.19 (1H, s), 2.76 (3H, d). refluxed for 5 h evaporated Water was added the mixture extracted with ethyl acetate dried over sodium sulphate evaporated

反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2-Fluorobenzonitrile (10.0 g, 82.8 mmol) was dissolved in acetonitrile (100 ml), and 40% aqueous methylamine solution (200 ml) was added thereto, followed by stirring at 60° C. overnight. 40% aqueous methylamine solution (100 ml) was further added thereto, followed by stirring at 60° C. for 9 hours. The reaction mixture was concentrated under reduced pressure, then water was added to the resulting residue, the mixture was extracted with chloroform. After the organic layer was dried (over anhydrous magnesium sulfate), the drying agent was filtered off, and the organic layer was concentrated under reduced pressure. The resulting oily substances were purified by silica gel column chromatography (the substances were eluted with an increasing concentration of chloroform from chloroform/hexane=1/2 to chloroform/hexane=1/1) to give the title compound (5.38 g, 49%). by stirring at 60° C. for 9 hours The reaction mixture was concentrated under reduced pressure water was added to the resulting residue the mixture was extracted with chloroform After the organic layer was dried (over anhydrous magnesium sulfate) the drying agent was filtered off the organic layer was concentrated under reduced pressure The resulting oily substances were purified by silica gel column chromatography (the substances were eluted with an increasing concentration of chloroform from chloroform/hexane=1/2 to chloroform/hexane=1/1)