5-甲基-1,4-氧氮杂环庚烷盐酸盐

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

实验步骤: Preparation of 6-(4-[1,2,4]oxadiazol-3-yl-phenyl) -[1,4]oxazepane was performed by the same procedure as that of 5-methyl-[1,4]oxazepane hydrochloride except for utilizing 4-benzyl-6-(4-[1,2,4]oxadiazol-3-yl-phenyl)-[1,4]oxazepane instead of 4-benzyl-5-methyl-[1,4]oxazepane. 6-(4-[1,2,4]Oxadiazol-3-yl-phenyl)-[1,4]oxazepane hydrochloride was obtained as white solid (0.13 g, 0.45 mmol, 86%).

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

实验步骤: Preparation of 6-(4-[1,2,4]oxadiazol-3-yl-phenyl) -[1,4]oxazepane was performed by the same procedure as that of 5-methyl-[1,4]oxazepane hydrochloride except for utilizing 4-benzyl-6-(4-[1,2,4]oxadiazol-3-yl-phenyl)-[1,4]oxazepane instead of 4-benzyl-5-methyl-[1,4]oxazepane. 6-(4-[1,2,4]Oxadiazol-3-yl-phenyl)-[1,4]oxazepane hydrochloride was obtained as white solid (0.13 g, 0.45 mmol, 86%).

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

实验步骤: 5-Phenyl-[1,4]oxazepane hydrochloride was prepared by the same procedure as that of 5-methyl-[1,4]oxazepane hydrochloride except for utilizing 4-benzyl-5-phenyl-[1,4]oxazepane instead of 4-benzyl-5-methyl-[1,4]oxazepane. Then 5-phenyl-[1,4]oxazepane hydrochloride was obtained as white solid (0.14 g, 0.65 mmol, 73%).

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

实验步骤: 5-Phenyl-[1,4]oxazepane hydrochloride was prepared by the same procedure as that of 5-methyl-[1,4]oxazepane hydrochloride except for utilizing 4-benzyl-5-phenyl-[1,4]oxazepane instead of 4-benzyl-5-methyl-[1,4]oxazepane. Then 5-phenyl-[1,4]oxazepane hydrochloride was obtained as white solid (0.14 g, 0.65 mmol, 73%).

反应条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of 5-methyl-[1,4]oxazepane hydrochloride (0.08 g, 0.50 mmol) and 2-chloro-3-methyl-6-(pyrimidin-4-yl)-3H-pyrimidin-4-one (0.09 g, 0.40 mmol) in tetrahydrofuran (2 mL) in a sealed tube was added triethylamine (0.14 mL) at room temperature. The mixture was heated to 150° C. under microwave irradiation and stirred for 30 min. After cooling to room temperature, the reaction mixture was poured into water and extracted with chloroform. The extracts were dried over anhydrous sodium sulfate and concentrated. The residue was purified by flash column chromatography on silica gel (chloroform/methanol=10/1 as an eluant) to yield 2-(5-methyl-[1,4]oxazepane-4-yl)-3-methyl-6-pyrimidin-4-yl-3H-pyrimidin-4-one (0.03 g, 0.09 mmol, 22%) as a white solid. After cooling to room temperature extracted with chloroform The extracts were dried over anhydrous sodium sulfate concentrated The residue was purified by flash column chromatography on silica gel (chloroform/methanol=10/1 as an eluant)

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

实验步骤: To a solution of 4-benzyl-5-methyl-[1,4]oxazepane (0.30 g, 1.4 mmol) in 1,2-dichloroethane (3 mL) was added chloroethyl chloroformate (0.56 mL, 7 mmol) at room temperature. The mixture was refluxed for 10 hours and concentrated. The resulting residue was dissolved in methanol (5 mL) and the solution was refluxed for one hour. After concentration, the residual material was triturated, washed with ethyl acetate and collected by filtration to afford 5-methyl-[1,4]oxazepane hydrochloride (0.16 g, 1.1 mmol, 76%) as a white solid. The mixture was refluxed for 10 hours concentrated The resulting residue was dissolved in methanol (5 mL) the solution was refluxed for one hour After concentration the residual material was triturated washed with ethyl acetate collected by filtration

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

实验步骤: To a solution of 4-benzyl-5-methyl-[1,4]oxazepane (0.30 g, 1.4 mmol) in 1,2-dichloroethane (3 mL) was added chloroethyl chloroformate (0.56 mL, 7 mmol) at room temperature. The mixture was refluxed for 10 hours and concentrated. The resulting residue was dissolved in methanol (5 mL) and the solution was refluxed for one hour. After concentration, the residual material was triturated, washed with ethyl acetate and collected by filtration to afford 5-methyl-[1,4]oxazepane hydrochloride (0.16 g, 1.1 mmol, 76%) as a white solid. The mixture was refluxed for 10 hours concentrated The resulting residue was dissolved in methanol (5 mL) the solution was refluxed for one hour After concentration the residual material was triturated washed with ethyl acetate collected by filtration

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

实验步骤: Preparation of 6-(4-[1,2,4]oxadiazol-3-yl-phenyl) -[1,4]oxazepane was performed by the same procedure as that of 5-methyl-[1,4]oxazepane hydrochloride except for utilizing 4-benzyl-6-(4-[1,2,4]oxadiazol-3-yl-phenyl)-[1,4]oxazepane instead of 4-benzyl-5-methyl-[1,4]oxazepane. 6-(4-[1,2,4]Oxadiazol-3-yl-phenyl)-[1,4]oxazepane hydrochloride was obtained as white solid (0.13 g, 0.45 mmol, 86%).

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

实验步骤: 5-Phenyl-[1,4]oxazepane hydrochloride was prepared by the same procedure as that of 5-methyl-[1,4]oxazepane hydrochloride except for utilizing 4-benzyl-5-phenyl-[1,4]oxazepane instead of 4-benzyl-5-methyl-[1,4]oxazepane. Then 5-phenyl-[1,4]oxazepane hydrochloride was obtained as white solid (0.14 g, 0.65 mmol, 73%).

反应条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of 5-methyl-[1,4]oxazepane hydrochloride (0.08 g, 0.50 mmol) and 2-chloro-3-methyl-6-(pyrimidin-4-yl)-3H-pyrimidin-4-one (0.09 g, 0.40 mmol) in tetrahydrofuran (2 mL) in a sealed tube was added triethylamine (0.14 mL) at room temperature. The mixture was heated to 150° C. under microwave irradiation and stirred for 30 min. After cooling to room temperature, the reaction mixture was poured into water and extracted with chloroform. The extracts were dried over anhydrous sodium sulfate and concentrated. The residue was purified by flash column chromatography on silica gel (chloroform/methanol=10/1 as an eluant) to yield 2-(5-methyl-[1,4]oxazepane-4-yl)-3-methyl-6-pyrimidin-4-yl-3H-pyrimidin-4-one (0.03 g, 0.09 mmol, 22%) as a white solid. After cooling to room temperature extracted with chloroform The extracts were dried over anhydrous sodium sulfate concentrated The residue was purified by flash column chromatography on silica gel (chloroform/methanol=10/1 as an eluant)

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

实验步骤: To a solution of 4-benzyl-5-methyl-[1,4]oxazepane (0.30 g, 1.4 mmol) in 1,2-dichloroethane (3 mL) was added chloroethyl chloroformate (0.56 mL, 7 mmol) at room temperature. The mixture was refluxed for 10 hours and concentrated. The resulting residue was dissolved in methanol (5 mL) and the solution was refluxed for one hour. After concentration, the residual material was triturated, washed with ethyl acetate and collected by filtration to afford 5-methyl-[1,4]oxazepane hydrochloride (0.16 g, 1.1 mmol, 76%) as a white solid. The mixture was refluxed for 10 hours concentrated The resulting residue was dissolved in methanol (5 mL) the solution was refluxed for one hour After concentration the residual material was triturated washed with ethyl acetate collected by filtration