N-methyl-N'-phenylethane-1,2-diamine

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: Here, 3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-1-chloropropane (9 g, 0.0336 mol) is heated to 130° C. for 30 minutes with N-(2-phenylaminoethyl)-methylamine (11 g, 0.073 mol). After cooling, the reaction mixture is distributed between water and diethylether. The organic phase is separated, dried over sodium sulfate and concentrated by evaporation. The residue is recrystallized from toluene/petroleum ether. After cooling The organic phase is separated dried over sodium sulfate concentrated by evaporation The residue is recrystallized from toluene/petroleum ether

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: In a manner similar to preparation 1, react N-methyl-N'-phenyl-1,2-ethanediamine with 2,3-dibromopropanamide to obtainthe title compound. In a manner similar to preparation 1

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

実験手順: In a manner similar to preparation 1, react N-methyl-N'-phenyl-1,2-ethanediamine with 2,3-dibromopropanamide to obtainthe title compound. In a manner similar to preparation 1

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

実験手順: Here, 3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-1-chloropropane (9 g, 0.0336 mol) is heated to 130° C. for 30 minutes with N-(2-phenylaminoethyl)-methylamine (11 g, 0.073 mol). After cooling, the reaction mixture is distributed between water and diethylether. The organic phase is separated, dried over sodium sulfate and concentrated by evaporation. The residue is recrystallized from toluene/petroleum ether. After cooling The organic phase is separated dried over sodium sulfate concentrated by evaporation The residue is recrystallized from toluene/petroleum ether

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

実験手順: Here, 3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-1-chloropropane (9 g, 0.0336 mol) is heated to 130° C. for 30 minutes with N-(2-phenylaminoethyl)-methylamine (11 g, 0.073 mol). After cooling, the reaction mixture is distributed between water and diethylether. The organic phase is separated, dried over sodium sulfate and concentrated by evaporation. The residue is recrystallized from toluene/petroleum ether. After cooling The organic phase is separated dried over sodium sulfate concentrated by evaporation The residue is recrystallized from toluene/petroleum ether

反応条件: temp:170.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of aniline hydrochloride (13.0 g, 0.10 mole), 3-methyl-2-oxazolidinone (11.0 g, 0.109 mole) and 35 ml of 2-(2-methoxyethoxy)ethanol was heated to 170° C. in an oil bath. The reaction mixture became homogenous and carbon dioxide evolution occurred on heating. After 17 hours, the reaction was allowed to cool to room temperature. After a workup procedure similar to that described in Example 1 and distillation at 105° C. to 110° C. (0.4 mm), an 81 percent distilled yield of the product was obtained as a clear liquid. Product confirmation was made by the use of spectra evidence. on heating to cool to room temperature After a workup procedure similar to that described in Example 1 and distillation at 105° C. to 110° C. (0.4 mm) an 81 percent distilled yield of the product was obtained as a clear liquid

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

実験手順: In a manner similar to preparation 1, react N-methyl-N'-phenyl-1,2-ethanediamine with 2,3-dibromopropanamide to obtain the title compound. In a manner similar to preparation 1

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

実験手順: In a manner similar to preparation 1, react N-methyl-N'-phenyl-1,2-ethanediamine with 2,3-dibromopropanamide to obtainthe title compound. In a manner similar to preparation 1

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

実験手順: Here, 3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-1-chloropropane (9 g, 0.0336 mol) is heated to 130° C. for 30 minutes with N-(2-phenylaminoethyl)-methylamine (11 g, 0.073 mol). After cooling, the reaction mixture is distributed between water and diethylether. The organic phase is separated, dried over sodium sulfate and concentrated by evaporation. The residue is recrystallized from toluene/petroleum ether. After cooling The organic phase is separated dried over sodium sulfate concentrated by evaporation The residue is recrystallized from toluene/petroleum ether