N-methyl-2-phenoxyethanamine

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:

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: The title compound is prepared from [3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-1-chloropropane and N-(2-phenyloxyethyl)-methylamine analogously to Example 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 (18.5 g, 0.0623 mol) is heated to 110° C. for 2 hours in an autoclave with N-(2-phenyloxyethyl)-methylamine (10.3 g, 0.0623 mol) and triethylamine (8.7 ml, 0.062 mol). After cooling, the reaction mixture is distributed between methylene chloride and water, the organic phase is separated off, dried over sodium sulfate and concentrated by evaporation. The residue is purified by chromatography on silica gel (eluant: methylene chloride/methanol=9/1). The base thus obtained is converted into the hydrochloride in the usual way. After cooling the organic phase is separated off dried over sodium sulfate concentrated by evaporation The residue is purified by chromatography on silica gel (eluant: methylene chloride/methanol=9/1) The base thus obtained

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

実験手順: A mixture of 2,3-dichloropyrazine (6.64 g, 44.6mmol) and N-methyl-N-(2-phenoxyethyl)amine* (4.5 g, 29.8 mmol) in DMF (5 mL) was placed in a sealed Pyrex tube and heated in a microwave oven (Labwell MW10) for 1×2 min followed by 2×1 min at 75W. The mixture was concentrated and the resulting oil was purified by column chromatography on silica using hexane/EtOAc (95:5 followed by 93:7) to give 5.56 g (71%) of the title product as a colorless oil. HRMS m/z calcd for C13H14ClN3O (M)+ 263.0825, found 263.0824. was placed in a sealed Pyrex tube heated in a microwave oven (Labwell MW10) for 1×2 min The mixture was concentrated the resulting oil was purified by column chromatography on silica

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

実験手順: A mixture of 2,3-dichloropyrazine (6.64 g, 44.6mmol) and N-methyl-N-(2-phenoxyethyl)amine* (4.5 g, 29.8 mmol) in DMF (5 mL) was placed in a sealed Pyrex tube and heated in a microwave oven (Labwell MW10) for 1×2 min followed by 2×1 min at 75W. The mixture was concentrated and the resulting oil was purified by column chromatography on silica using hexane/EtOAc (95:5 followed by 93:7) to give 5.56 g (71%) of the title product as a colorless oil. HRMS m/z calcd for C13H14ClN3O (M)+ 263.0825, found 263.0824. was placed in a sealed Pyrex tube heated in a microwave oven (Labwell MW10) for 1×2 min The mixture was concentrated the resulting oil was purified by column chromatography on silica

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

実験手順: A mixture of 2,3-dichloropyrazine (6.64 g, 44.6mmol) and N-methyl-N-(2-phenoxyethyl)amine* (4.5 g, 29.8 mmol) in DMF (5 mL) was placed in a sealed Pyrex tube and heated in a microwave oven (Labwell MW10) for 1×2 min followed by 2×1 min at 75W. The mixture was concentrated and the resulting oil was purified by column chromatography on silica using hexane/EtOAc (95.5 followed by 93:7) to give 5.56 g (71%) of the title product as a colorless oil. HRMS m/z calcd for C13H14ClN3O (M)+263.0825, found 263.0824 was placed in a sealed Pyrex tube heated in a microwave oven (Labwell MW10) for 1×2 min The mixture was concentrated the resulting oil was purified by column chromatography on silica

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

実験手順: The title compound is prepared from [3-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-1-chloropropane and N-(2-phenyloxyethyl)-methylamine analogously to Example 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 (18.5 g, 0.0623 mol) is heated to 110° C. for 2 hours in an autoclave with N-(2-phenyloxyethyl)-methylamine (10.3 g, 0.0623 mol) and triethylamine (8.7 ml, 0.062 mol). After cooling, the reaction mixture is distributed between methylene chloride and water, the organic phase is separated off, dried over sodium sulfate and concentrated by evaporation. The residue is purified by chromatography on silica gel (eluant: methylene chloride/methanol=9/1). The base thus obtained is converted into the hydrochloride in the usual way. After cooling the organic phase is separated off dried over sodium sulfate concentrated by evaporation The residue is purified by chromatography on silica gel (eluant: methylene chloride/methanol=9/1) The base thus obtained

反応条件: temp:0.00; pressure:0.00; stir: