7-(4-oxime-3-amino-1-piperidine) quinoline carboxylic acid derivative and method for making same
An amino protecting group, carboxylic acid technology, applied in the field of medicinal chemistry, can solve the problems of poor water solubility, limited wide application, limited application scope and the like
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Embodiment 1
[0171] Embodiment 1, 4-hydroxyl-1-benzyl-piperidine-3-carboxylic acid ethyl ester
[0172] Add triethylamine (1.4ml) dropwise to a solution of ethyl 1-benzyl-4-oxo-piperidine-3-carboxylate (6.0g, 20mmol) and 95% ethanol (20ml) under ice-cooling , then added potassium borohydride (1.7g, 27mmol) in batches, poured into water after reacting for 2h, extracted with dichloromethane, washed with water, dried, and concentrated under reduced pressure to give 3.1g of light yellow oil with a yield of 58.4%.
[0173] 1 H NMR (300MHz, CDCl 3 +D 2 O) δ ppm: 1.298 (3H, s, CH 3 ), 1.782~1.915 (2H, m, C 5 -2H), 2.357~2.791 (5H, m, C 2 -2H,C 3 -1H,C 6 -2H), 3.727~4.391 (5H, m, phCH 2 , C 4 -1H,CH 2 CH 3 ), 7.132~7.268 (5H, m, ph-5H).
[0174] MS (FAB, m / z): 264 (M + +1).
Embodiment 2
[0175] Embodiment 2, 4-hydroxyl-1-benzyl-piperidine-3-carboxamide
[0176] Compound of Example 1 (5.5 g, 13.8 mmol) was added ammonia water (20 ml), stirred at room temperature for 12 h, concentrated under reduced pressure, dissolved in chloroform, washed with water, dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure to obtain 4.8 g of a colorless oily product , yield 65.4%.
[0177] 1 HNMR (300MHz, DMSO+D 2 O) δ ppm: 1.592~1.599 (2H, s, C 5 -2H), 2.343~2.523 (5H, m, C 2 -2H,C 3 -1H,C 6 -2H), 3.436~3.499 (2H, m, ph CH 2 ), 4.020 (1H, s, C 4 -1H), 4.821 (1H, s, OH), 6.953 (1H, s, NH), 7.222~7.331 (5H, m, ph-5H), 7.382 (1H, s, NH).
[0178] MS (FAB, m / z): 235 (M + +1).
Embodiment 3
[0179] Embodiment 3, 3-amino-4-hydroxyl-1-benzyl-piperidine
[0180] Method one: add sodium hydroxide (6.8g, 0.17mol) in batches to the mixed solution of 12% sodium hypochlorite (25.9ml) and water (5ml) under ice-cooling, add embodiment 2 compound (3.0g , 12.9mmol), stirring and reacting at room temperature for half an hour, raising the temperature to 70°C for 3h, lowering to room temperature, adjusting pH=9, extracting with dichloromethane, washing with water, drying, and evaporating to dryness to obtain 1.33g of a colorless oil, yield 50%.
[0181] Method 2: The compound of Example 2 (3.0g, 12.9mmol) was dissolved in 6% NaOH solution (10ml), and 12% sodium hypochlorite (25.9ml) was added dropwise under ice-cooling conditions, stirred at room temperature for 0.5h, and heated to React at 70°C for 3 hours, lower to room temperature, adjust pH to about 9, extract with dichloromethane, wash with water, dry, and evaporate the solvent to give 1.38 g of a colorless oil. Yield 52%....
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