2-哌啶羧酸,1,1-二甲基乙基酯,(2S)

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

实验步骤: To a solution of (S)-piperidine-2-carboxylic acid tert-butyl ester (M. Egbertson and S. J. Danishefsky, J. Org. Chem., 1989, 54, 1, 11-12) (5.78 g, 31.2 mmol) in CH3CN (30 mL) at 0° C. was added DMAP (763 mg, 6.2 mmol) followed by BOC2O (10.22 g, 46.8 mmol). The reaction mixture was allowed to warm to room temperature and stirred for 20 h. The solvents were evaporated under reduced pressure and the residue was purified by flash chromatography (10% ethyl acetate in hexane). The title compound was obtained as a colourless oil which crystallized upon standing (8.33 g, 94%): 1H NMR (400 MHz, CDCl3) δ 1.21-1.32 (2H, m), 1.47-1.48 (18H, 2 s), 1.59-1.72 (3H, m), 2.18 (1H, m), 2.85-3.00 (1H, m), 3.89-4.01 (1H, 2 d, J 11.9 Hz), 4.47-4.58 (1H, 2 br s). Method H: The solvents were evaporated under reduced pressure the residue was purified by flash chromatography (10% ethyl acetate in hexane)

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

实验步骤: To a solution of (S)-piperidine-2-carboxylic acid tert-butyl ester (M. Egbertson and S. J. Danishefsky, J. Org. Chem., 1989, 54, 1, 11-12) (5.78 g, 31.2 mmol) in CH3CN (30 mL) at 0° C. was added DMAP (763 mg, 6.2 mmol) followed by BOC2O (10.22 g, 46.8 mmol). The reaction mixture was allowed to warm to room temperature and stirred for 20 h. The solvents were evaporated under reduced pressure and the residue was purified by flash chromatography (10% ethyl acetate in hexane). The title compound was obtained as a colourless oil which crystallized upon standing (8.33 g, 94%): 1H NMR (400 MHz, CDCl3) δ 1.21-1.32 (2H, m), 1.47-1.48 (18H, 2 s), 1.59-1.72 (3H, m), 2.18 (1H, m), 2.85-3.00 (1H, m), 3.89-4.01 (1H, 2 d, J 11.9 Hz), 4.47-4.58 (1H, 2 br s). Method H: The solvents were evaporated under reduced pressure the residue was purified by flash chromatography (10% ethyl acetate in hexane)

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

实验步骤: To a solution of (S)-piperidine-2-carboxylic acid tert-butyl ester (M. Egbertson and S. J. Danishefsky, J. Org. Chem., 1989, 54, 1, 11-12) (5.78 g, 31.2 mmol) in CH3CN (30 mL) at 0° C. was added DMAP (763 mg, 6.2 mmol) followed by BOC2O (10.22 g, 46.8 mmol). The reaction mixture was allowed to warm to room temperature and stirred for 20 h. The solvents were evaporated under reduced pressure and the residue was purified by flash chromatography (10% ethyl acetate in hexane). The title compound was obtained as a colorless oil which crystallized upon standing (8.33 g, 94%): 1H NMR (400 MHz, CDCl3) δ 1.21-1.32 (2H, m), 1.47-1.48 (18H, 2s), 1.59-1.72 (3H, m), 2.18 (1H, m), 2.85-3.00 (1H, m), 3.89-4.01 (1H, 2d, J 11.9 Hz), 4.47-4.58 (1H, 2br s). The solvents were evaporated under reduced pressure the residue was purified by flash chromatography (10% ethyl acetate in hexane)

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

实验步骤: To a solution of (S)-piperidine-2-carboxylic acid tert-butyl ester (M. Egbertson and S. J. Danishefsky, J. Org. Chem., 1989, 54, 1, 11-12) (5.78 g, 31.2 mmol) in CH3CN (30 mL) at 0° C. was added DMAP (763 mg, 6.2 mmol) followed by BOC2O (10.22 g, 46.8 mmol). The reaction mixture was allowed to warm to room temperature and stirred for 20 h. The solvents were evaporated under reduced pressure and the residue was purified by flash chromatography (10% ethyl acetate in hexane). The title compound was obtained as a colorless oil which crystallized upon standing (8.33 g, 94%): 1H NMR (400 MHz, CDCl3) δ 1.21-1.32 (2H, m), 1.47-1.48 (18H, 2s), 1.59-1.72 (3H, m), 2.18 (1H, m), 2.85-3.00 (1H, m), 3.89-4.01 (1H, 2d, J 11.9 Hz), 4.47-4.58 (1H, 2br s). The solvents were evaporated under reduced pressure the residue was purified by flash chromatography (10% ethyl acetate in hexane)

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

实验步骤: To a solution of (S)-piperidine-2-carboxylic acid tert-butyl ester (M. Egbertson and S. J. Danishefsky, J. Org. Chem., 1989, 54, 1, 11-12) (5.78 g, 31.2 mmol) in CH3CN (30 mL) at 0° C. was added DMAP (763 mg, 6.2 mmol) followed by BOC2O (10.22 g, 46.8 mmol). The reaction mixture was allowed to warm to room temperature and stirred for 20 h. The solvents were evaporated under reduced pressure and the residue was purified by flash chromatography (10% ethyl acetate in hexane). The title compound was obtained as a colorless oil which crystallized upon standing (8.33 g, 94%): 1H NMR (400 MHz, CDCl3) δ 1.21-1.32 (2H, m), 1.47-1.48 (18H, 2s), 1.59-1.72 (3H, m), 2.18 (1H, m), 2.85-3.00 (1H, m), 3.89-4.01 (1H, 2d, J 11.9 Hz), 4.47-4.58 (1H, 2br s). The solvents were evaporated under reduced pressure the residue was purified by flash chromatography (10% ethyl acetate in hexane)

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

实验步骤: To a solution of (S)-piperidine-2-carboxylic acid tert-butyl ester (M. Egbertson and S. J. Danishefsky, J. Org. Chem., 1989, 54, 1, 11-12) (5.78 g, 31.2 mmol) in CH3CN (30 mL) at 0° C. was added DMAP (763 mg, 6.2 mmol) followed by BOC2O (10.22 g, 46.8 mmol). The reaction mixture was allowed to warm to room temperature and stirred for 20 h. The solvents were evaporated under reduced pressure and the residue was purified by flash chromatography (10% ethyl acetate in hexane). The title compound was obtained as a colourless oil which crystallized upon standing (8.33 g, 94%): 1H NMR (400 MHz, CDCl3) δ 1.21-1.32 (2H, m), 1.47-1.48 (18H, 2 s), 1.59-1.72 (3H, m), 2.18 (1H, m), 2.85-3.00 (1H, m), 3.89-4.01 (1H, 2 d, J=11.9 Hz), 4.47-4.58 (1H, 2br s). The solvents were evaporated under reduced pressure the residue was purified by flash chromatography (10% ethyl acetate in hexane)