Quinuclidinol derivatives as muscarinic receptor antagonists
A compound and alkyl technology, applied in the field of quinol derivatives as muscarinic receptor antagonists, can solve the problems of insufficient treatment, short duration of action, inconvenience to patients and the like
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Embodiment 1
[0408] Example 1: (3R)-1-(3-phenoxypropyl)-3-[(2-phenyl-2-(piperidin-1-yl)propionyl)oxy]-1-bromide Nitrobicyclo[2.2.2]octane
[0409]
[0410] a) Methyl 2-phenyl-2-(piperidin-1-yl)propionate
[0411]
[0412]A solution of methyl 2-bromo-2-phenylpropanoate (1 g) in acetonitrile (30 mL) was treated with piperidine (1 mL). The solution was stirred and heated at reflux for 3 hours, then concentrated to dryness. The residue was purified by flash column chromatography on silica gel using diethyl ether / isohexane (3:7) to give the racemic subtitle compound as a colorless oil (0.8 g).
[0413] 1 H NMR (400MHz, CDCl 3 ( 2H, m,), 1.60-1.51 (4H, m,), 1.56 (3H, s), 1.48-1.39 (2H, m).
[0414] b) 2-Phenyl-2-(piperidin-1-yl)propanoic acid (3R)-1-azabicyclo[2.2.2]oct-3-yl ester
[0415]
[0416] Under a nitrogen atmosphere, while stirring, add (3R)-quinuclidin-3-ol (available from AcrosOrganics 1 A solution of methyl 2-phenyl-2-(piperidin-1-yl)propionate (Example 1a, 0.6 g) i...
Embodiment 2
[0423] Example 2: Bromide (3R)-1-[2-(isoxazol-3-ylamino)-2-oxoethyl]-3-{[(2S)-2-phenyl-2-( Piperidin-1-yl)propionyl]oxy}-1-azoniumbicyclo[2.2.2]octane (isomer 1)
[0424]
[0425] a) Methyl 2-phenyl-2-(piperidin-1-yl)propanoate (enantiomers 1 and 2)
[0426]
[0427] Racemic methyl 2-phenyl-2-(piperidin-1-yl)propanoate was synthesized according to the procedure described in Example 1a. Separation of the enantiomeric mixture by chiral HPLC using an isocratic system of 80% isohexane / ethanol and a chiracel OJ-H column afforded the two enantiomers (2S)-2-phenyl-2- Methyl (piperidin-1-yl)propionate (isomer 1) and methyl (2R)-2-phenyl-2-(piperidin-1-yl)propionate (isomer 2).
[0428] Methyl (2S)-2-phenyl-2-(piperidin-1-yl)propionate (isomer 1)
[0429]
[0430] Chiral HPLC 80:20 isohexane:ethanol (isocratic). Chiracel OJ-H 4.6mmx50mm
[0431] The retention time is 1.09min.
[0432] 1 H NMR (400MHz, CDCl 3 )δ7.56-7.49 (2H, m), 7.35-7.20 (3H, m), 3.68 (3H, s), 2.54-2....
Embodiment 3
[0448] Example 3: Bromide (3R)-1-[2-(isoxazol-3-ylamino)-2-oxoethyl]-3-{[(2R)-2-phenyl-2-( Piperidin-1-yl)propionyl]oxy}-1-azoniumbicyclo[2.2.2]octane (isomer 2)
[0449]
[0450] a) (2R)-2-Phenyl-2-(piperidin-1-yl)propanoic acid (3R)-1-azabicyclo[2.2.2]oct-3-yl ester (isomer 2)
[0451]
[0452] The subtitle compound was followed the procedure described in Example 1b using (2R)-2-phenyl-2-(piperidin-1-yl)propanoic acid methyl ester (Example 2a, Isomer 2, 0.47g), ( 3R)-Quinuclidin-3-ol (0.6 g) and sodium hydride (175 mg, 60% dispersion in mineral oil) were prepared. The subtitle compound was isolated as a gum (450mg).
[0453] 1H NMR (400MHz, DMSO) δ7.58-7.50 (2H, m), 7.39-7.21 (3H, m), 4.70-4.60 (1H, m), 3.43-3.28 (1H, m), 3.13-3.01 (1H , m), 2.77-2.29 (7H, m), 1.83-1.76 (1H, m), 1.64-1.19 (14H, m).
[0454] Example 3: Bromide (3R)-1-[2-(isoxazol-3-ylamino)-2-oxoethyl]-3-{[(2R)-2-phenyl-2-( Piperidin-1-yl)propionyl]oxy}-1-azoniumbicyclo[2.2.2]octane (isomer 2)
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