5-Methylazepan-4-One Hydrochloride

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

实验步骤: Acetic anhydride (0.437 mL, 4.62 mmol) was added at 0° C. to a solution of 5-methyl-azepan-4-one hydrochloride (0.740 g, 3.08 mmol) in DCM (20 mL) and pyridine (0.25 mL, 3.08 mmol). The reaction mixture was stirred at RT for 8 hours before being partitioned between DCM and H2O. The organic layer was dried (Na2SO4), filtered, and evaporated. The crude residue was purified by SiO2 chromatography (100% EtOAc) to give 0.220 g of 1-acetyl-5-methyl-azepan-4-one (42% yield). before being partitioned between DCM and H2O The organic layer was dried (Na2SO4) filtered evaporated The crude residue was purified by SiO2 chromatography (100% EtOAc)

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

实验步骤: A solution of 4-methyl-5-oxo-azepane-1-carboxylic acid tert-butyl ester (700 mg, 3.083 mmol) was dissolved in 10% TFA in DCM (30 mL) and stirred at RT for 6 hours before being evaporated to give 0.74 g of 5-methyl-azepan-4-one hydrochloride. before being evaporated

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

实验步骤: A solution of 4-methyl-5-oxo-azepane-1-carboxylic acid tert-butyl ester (700 mg, 3.083 mmol) was dissolved in 10% TFA in DCM (30 mL) and stirred at RT for 6 hours before being evaporated to give 0.74 g of 5-methyl-azepan-4-one hydrochloride. before being evaporated

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

实验步骤: Acetic anhydride (0.437 mL, 4.62 mmol) was added at 0° C. to a solution of 5-methyl-azepan-4-one hydrochloride (0.740 g, 3.08 mmol) in DCM (20 mL) and pyridine (0.25 mL, 3.08 mmol). The reaction mixture was stirred at RT for 8 hours before being partitioned between DCM and H2O. The organic layer was dried (Na2SO4), filtered, and evaporated. The crude residue was purified by SiO2 chromatography (100% EtOAc) to give 0.220 g of 1-acetyl-5-methyl-azepan-4-one (42% yield). before being partitioned between DCM and H2O The organic layer was dried (Na2SO4) filtered evaporated The crude residue was purified by SiO2 chromatography (100% EtOAc)

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

实验步骤: A solution of 4-methyl-5-oxo-azepane-1-carboxylic acid tert-butyl ester (700 mg, 3.083 mmol) was dissolved in 10% TFA in DCM (30 mL) and stirred at RT for 6 hours before being evaporated to give 0.74 g of 5-methyl-azepan-4-one hydrochloride. before being evaporated