Fused bicyclic-N-bridged-heteroaromatic carboxamides for the treatment of disease
a carboxamide and bicyclic technology, applied in the field of nicotinic acetylcholine receptors, can solve the problems of limiting the functional assays that can be used, the receptor is rapidly inactivated, and the target is a difficult target for testing
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example 1
N-[(3R)-1-azabicyclo[2.2.2]oct-3-yl]pyrrolo[1,2-c]pyrimidine-3-carboxamide hydrochloride
[1071]
[1072] Pyrrolo[1,2-c]pyrimidine-3-carboxylic acid hydrochloride (0.33 g, 1.66 mmol) and TEA (2.0 mL, 14.35 mmol) are dissolved in 15 mL THF. Diphenylphosphinic chloride (0.47 g, 1.99 mmol) is added dropwise. After 1h, (R)-(+)-3-aminoquinuclidine dihydrochloride is added and the reaction is allowed to stir at RT. After 1day, 1N NaOH is added and the mixture is extracted with CHCl3. The combined organic layers are dried (MgSO4), filtered and concentrated. The residue is purified by chromatography (Biotage 40S, 90:9:1 CHCl3 / MeOH / NH4OH) to afford 0.45 g (100%) of product. The hydrochloride salt is prepared and recrystallized from CH3CN / Et2O. HRMS (FAB) calcd for C15H18N4O+H 271.1555, found 271.1559.
example 2
N-[(2S,3R)-2-methyl-1-azabicyclo[2.2.2]oct-3-yl]pyrrolo[1,2-c]pyrimidine-3-carboxamide hydrochloride
[1073]
[1074] Pyrrolo[1,2-c]pyrimidine-3-carboxylic acid hydrochloride (0.16 g, 0.82 mmol), HATU (0.47 g, 1.22 mmol) and 2-methyl-2.2.2-Amine (0.21 g, 1.0 mmol) are suspended in 15 mL CH3CN. DEA (1.4 mL, 8.0 mmol) is added dropwise. After 2 days, the solvent is removed and the residue is taken up in 1N NaOH and CHCl3. The aqueous layer is extracted with CHCl3, dried (MgSO4), filtered and concentrated. The residue is purified by chromatography (Biotage 40S, 90:9:1 CHCl3 / MeOH / NH4OH), and the hydrochloride salt is prepared and recrystallized from CH3CN / Et2O to provide 0.059 g (23%) of the product. HRMS (FAB) calcd for C16H20N4O+H 285.1715, found 285.1717.
example 3
N-[(3R,5R)-1-azabicyclo[3.2.1]oct-3-yl]pyrrolo[1,2-c]pyrimidine-3-carboxamide dihydrochloride
[1075]
[1076] A mixture of exo-3R,5R-[3.2.1]-Amine (0.221 g, 1.11 mmol), pyrrolo[1,2-c]pyrimidine-3-carboxylic acid hydrochloride (0.220 g, 1.11 mmol), THF (18 mL), DIEA (0.77 mL, 4.4 mmol), and DMF (4 mL) is cooled in an ice bath and treated with HATU (0.426 g, 1.12 mmol). The mixture is allowed to warm to RT overnight and is evaporated. The residue is purified by flash column chromatography (1:9:90; conc. NH4OH—MeOH—CHCl3). The dihydrochloride salt is formed and triturated with EtOH / Et2O to yield the desired product (0.360 g, 94%). MS (ESI) for C15H18N4O—(HCl)2 (MH)+m / z=270.
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