Intermediate for heterocyclic compound in preparing rotamase inhibitor
A technology of compound and cycloalkyl, applied in the direction of active ingredients of heterocyclic compounds, drug combination, organic chemistry, etc., can solve the problem of unclear mechanism of neurotrophic effect
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Embodiment 1
[0161] (2S)-1-(1,3-Benzo Oxazole -2-yl)-N 2 -[(3R)-1-Benzylpyrrolidin-3-yl]-2-
[0162] piperidine carboxamide
[0163]
[0164] Triethylamine (0.167 ml) was added to (2S)-1-(1,3-benzoxazol-2-yl)-2-piperidinecarboxylic acid (100 mg) [see Preparation 3], 1-hydroxybenzene Triazole hydrate (60.4 mg), (3R)-1-benzylpyrrolidin-3-ylamine (78.7 mg) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiene Amine hydrochloride (85.4mg) in dichloromethane (30ml) solution. The reaction mixture was stirred at room temperature for 18 hours, then the mixture was diluted with water and the organic phase was separated, dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The crude product was purified by silica gel column chromatography, eluting with a solvent gradient of 50:50:0 → 25:75:0 → 20:80:1 (volume ratio) hexane: ethyl acetate: 0.88 ammonia water to obtain ( 2S)-1-(1,3-Benzoxazol-2-yl)-N2 -[(3R)-1-Benzylpyrrolidin-3-yl]-2-piperidinecarboxamid...
Embodiment 2
[0169] (2S)-1-(1,3-Benzo Oxazole -2-yl)-N 2 -[(3S)-1-Benzylpyrrolidin-3-yl]-2-
[0170] piperidine carboxamide
[0171]
preparation example 3
[0172] The title compound was obtained from (2S)-1-(1,3-benzoxazol-2-yl)-2-piperidinecarboxylic acid [see Preparation 3] and (3S)-1- Benzylpyrrolidin-3-ylamine Preparation. The crude product was purified by column chromatography on silica gel, eluting with a solvent gradient of 50:50:1→20:80:1 (by volume) hexane:ethyl acetate:0.88 ammonia in 10% increments. The product was further purified by recrystallization from ethyl acetate: hexanes to afford (2S)-1-(1,3-benzoxazol-2-yl)-N as a white solid 2 -[(3S)-1-Benzylpyrrolidin-3-yl]-2-piperidinecarboxamide.
[0173] 1 H-NMR (CDCl 3 )δ: 7.40(1H,d), 7.30(1H,m), 7.20(6H,s), 7.05(1H,t), 6.60(1H,d), 4.85(1H,s), 4.45(1H,bs ), 4.25(1H, d), 3.60(2H, s), 3.20(1H, t), 2.75(1H, m), 2.55(2H, m), 2.35(1H, m), 2.25(2H, m) , 1.80-1.50(4H, m), 1.30(2H, m).
[0174] Analysis: Found C, 71.00; H, 7.00; N, 13.80; C 24 h 28 N 4 o 2 Theoretical values for C, 71.26; H, 6.98; N, 13.85%.
[0175] Optical rotation: [◇] 25 D =-102.0° (c=0.1, m...
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