Serotonin 5-ht2b inhibitory compounds
A compound, piperidine technology, applied in the field of serotonin 5-HT2B inhibitory compounds, can solve the problem of hERG having no affinity
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[0324] The following examples provide a more detailed description of the process conditions for the preparation of compounds of the invention. It should be understood, however, that the invention is not intended to be limited to the details of the following modes of preparation, as fully described herein and claimed.
example 1
[0325] Example 1. (4-((1H-Imidazol-2-yl)amino)piperidin-1-yl)(4'-fluoro-[1,1'-biphenyl]-4-yl)methanone (Scheme 2 )
[0326]
[0327] step 1 . Preparation of tert-butyl 4-(1H-imidazol-2-ylamino)piperidine-1-carboxylate.
[0328] 4-Oxopiperidine-1-carboxylic acid tert-butyl ester (5g, 25.12mmol), 1H-imidazol-2-amine hydrochloride (4.48g, 37.68mmol), trimethylamine (10.31mL, 75.36mmol) and A mixture of titanium(IV) isopropoxide (15.22 mL, 50.24 mmol) was stirred in THF (100 mL) at 25°C overnight. Sodium cyanoborohydride (2.37 g, 37.68 mmol) and methanol (10 mL) were then added. The reaction mixture was maintained at 25°C for 4 hours. Water (100 mL) and ethyl acetate (100 mL) were added, the organic layer was separated and evaporated to give an oil. Purification by chromatography (5% methanol in DCM) afforded the title compound as a white solid.
[0329] step 2 . Preparation of 4-(1H-imidazol-2-amino)piperidine hydrochloride.
[0330] tert-Butyl 4-(1H-imidazol-2-ylami...
example 2
[0333] Example 2. (4-(1H-Imidazol-2-yl)piperidin-1-yl)(3'-(methylsulfonyl)-[1,1'-biphenyl]-4-yl)methanone (Scheme 3)
[0334]
[0335] step 1 . Preparation of methyl 3'-(methylthio)-[1,1'-biphenyl]-4-carboxylate
[0336] (3-Bromophenyl)(methyl)sulfonamide (1.5g, 7.38mmol) and (4-(methoxycarbonyl)phenyl)boronic acid (1.72g, 9.6mmol) in DMF (10mL) at 25°C Stir the solution, add K 3 PO 4 (4.69 g, 22.1 mmol). The reaction mixture was saturated with argon for 10 minutes. Add PdCl to it 2 (dppf)DCM (301 mg, 0.36 mmol) and stirred at 80°C for 16 hours. The reaction was monitored by TLC and LCMS. After the reaction was complete, it was diluted with water (100 mL) and extracted with ethyl acetate (2 x 100 mL). The organic portion was dried, concentrated, and the residue was purified by flash column chromatography (30% ethyl acetate in hexanes) to afford the title compound as a white solid.
[0337] step 2 . Preparation of methyl 3'-(methylsulfonyl)-[1,1'-biphenyl]-4-car...
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