tert-butyl N-[(3R)-1-methyl-2-oxopiperidin-3-yl]carbamate

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

实验步骤: A solution of (R)-tert-butyl 1-methyl-2-oxopiperidin-3-ylcarbamate (310 mg, 1.36 mmol) in 2,2,2-trifluoroethanol (4.95 mL, 67.9 mmol) was heated at 150° C. for 3 h under microwave assisted conditions. The solvent was evaporated to dryness and the crude residue was purified by SiO2 chromatography (11 g, CH2Cl2/MeOH/NH4OH, 100:0:0 to 94:5.7:0.3) to give 120 mg (69%) of (R)-3-amino-1-methyl-piperidin-2-one as a light yellow oil. The solvent was evaporated to dryness the crude residue was purified by SiO2 chromatography (11 g, CH2Cl2/MeOH/NH4OH, 100:0:0 to 94:5.7:0.3)

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

实验步骤: A solution of (R)-tert-butyl 1-methyl-2-oxopiperidin-3-ylcarbamate (310 mg, 1.36 mmol) in 2,2,2-trifluoroethanol (4.95 mL, 67.9 mmol) was heated at 150° C. for 3 h under microwave assisted conditions. The solvent was evaporated to dryness and the crude residue was purified by SiO2 chromatography (11 g, CH2Cl2/MeOH/NH4OH, 100:0:0 to 94:5.7:0.3) to give 120 mg (69%) of (R)-3-amino-1-methyl-piperidin-2-one as a light yellow oil. The solvent was evaporated to dryness the crude residue was purified by SiO2 chromatography (11 g, CH2Cl2/MeOH/NH4OH, 100:0:0 to 94:5.7:0.3)

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

实验步骤: To a solution of (R)-tert-butyl 2-oxopiperidin-3-ylcarbamate (642 mg, 3.00 mmol) in N,N-dimethylformamide (3 mL) at room temperature was added sodium hydride (132 mg, 3.3 mmol). The reaction mixture stirred for 30 min, then iodomethane (206 μL, 3.3 mmol) was added and stirring was continued for 1 h. The reaction mixture was poured into water (50 mL) and extracted with EtOAc (100 mL), using a continuous extractor apparatus overnight. The organic extract was evaporated to dryness under vacuum and the crude residue was purified by SiO2 chromatography (23 g, CH2Cl2/MeOH/NH4OH, 100:0:0 to 94:5.7:0.3) to give 310 mg (45%) of (R)-tert-butyl 1-methyl-2-oxopiperidin-3-ylcarbamate as a colorless viscous oil. stirring was continued for 1 h extracted with EtOAc (100 mL) a continuous extractor apparatus overnight The organic extract was evaporated to dryness under vacuum the crude residue was purified by SiO2 chromatography (23 g, CH2Cl2/MeOH/NH4OH, 100:0:0 to 94:5.7:0.3)

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

实验步骤: A solution of (R)-tert-butyl 1-methyl-2-oxopiperidin-3-ylcarbamate (310 mg, 1.36 mmol) in 2,2,2-trifluoroethanol (4.95 mL, 67.9 mmol) was heated at 150° C. for 3 h under microwave assisted conditions. The solvent was evaporated to dryness and the crude residue was purified by SiO2 chromatography (11 g, CH2Cl2/MeOH/NH4OH, 100:0:0 to 94:5.7:0.3) to give 120 mg (69%) of (R)-3-amino-1-methyl-piperidin-2-one as a light yellow oil. The solvent was evaporated to dryness the crude residue was purified by SiO2 chromatography (11 g, CH2Cl2/MeOH/NH4OH, 100:0:0 to 94:5.7:0.3)

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

实验步骤: To a solution of (R)-tert-butyl 2-oxopiperidin-3-ylcarbamate (642 mg, 3.00 mmol) in N,N-dimethylformamide (3 mL) at room temperature was added sodium hydride (132 mg, 3.3 mmol). The reaction mixture stirred for 30 min, then iodomethane (206 μL, 3.3 mmol) was added and stirring was continued for 1 h. The reaction mixture was poured into water (50 mL) and extracted with EtOAc (100 mL), using a continuous extractor apparatus overnight. The organic extract was evaporated to dryness under vacuum and the crude residue was purified by SiO2 chromatography (23 g, CH2Cl2/MeOH/NH4OH, 100:0:0 to 94:5.7:0.3) to give 310 mg (45%) of (R)-tert-butyl 1-methyl-2-oxopiperidin-3-ylcarbamate as a colorless viscous oil. stirring was continued for 1 h extracted with EtOAc (100 mL) a continuous extractor apparatus overnight The organic extract was evaporated to dryness under vacuum the crude residue was purified by SiO2 chromatography (23 g, CH2Cl2/MeOH/NH4OH, 100:0:0 to 94:5.7:0.3)