1-naphthyl alkylpiperidine derivative
A kind of alkyl, alkylene technology, applied in the field of 1-naphthyl alkyl piperidine derivatives, can solve the problem of no disclosure and teaching, enhancing MCH receptor antagonism and the like
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Embodiment 1
[0474] Example 1: 3-methoxy-N-[1-({7-[(2-methoxyethoxy)methyl]-2-naphthyl}methyl)piperidin-4-yl]benzene Synthesis of Formamide Hydrochloride
[0475] Step 1-1: Under nitrogen atmosphere, under ice cooling, to LiAlH 4 To a THF (1.25 L) suspension of (81.6 g) was added a THF (2.50 L) solution of dimethyl naphthalene-2,7-dicarboxylate (250 g), and the temperature was raised to room temperature. After stirring for 1 hour, ice cooling was performed again, and Na 2 SO 4 10H 2 O, stirred at room temperature for 15 minutes. The reaction solution was filtered through celite, washed with heated THF (12.0 L), and the filtrate was concentrated under reduced pressure. To the resulting bold was added CHCl 3 (1.00 L) was stirred for 10 minutes, and the solid was collected by filtration to obtain naphthalene-2,7-diyldimethanol (151 g, colorless solid).
[0476] 1 H NMR (200MHz, DMSO-d 6 , δ): 4.66(d, J=5.7Hz, 4H), 5.31(t, J=5.7Hz, 2H), 7.42(dd, J=8.6, 1.5Hz, 2H), 7.73-7.88(m, 4H) ; ...
Embodiment 2
[0487] Example 2: 3-methoxy-N-[1-({7-[(2-methoxyethoxy)methyl]-2-naphthyl}methyl)piperidin-4-yl]benzene Synthesis of formamide hydrobromide
[0488] To an EtOAc (10.0 mL) suspension of the compound (1.00 g) obtained in Step 1-5 was added 48% HBr aqueous solution (730 mg), followed by stirring at room temperature for 2.5 hours. The resulting solid was collected by filtration to obtain the title compound (1.09 g, colorless solid).
[0489] 1 H NMR (600MHz, CDCl 3, δ): 2.18-2.24(m, 2H), 2.53-2.63(m, 2H), 2.93-3.01(m, 2H), 3.43(s, 3H), 3.58-3.64(m, 4H), 3.68-3.71 (m, 2H), 3.84(s, 3H), 4.26-4.34(m, 1H), 4.37(d, J=5.0Hz, 2H), 4.76(s, 2H), 6.59(d, J=8.3Hz, 1H), 7.02-7.05(m, 1H), 7.28-7.33(m, 3H), 7.59-7.62(m, 1H), 7.82(dd, J=8.3, 1.8Hz, 1H), 7.87-7.90(m, 2H), 7.94(d, J=8.3Hz, 1H), 8.10(s, 1H), 11.62(brs, 1H); ESI / APCI MS m / z 463, [M(free)+H] + .
Embodiment 3
[0490] Example 3: Synthesis of 7-({4-[(3-methoxybenzoyl)amino]piperidin-1-yl}methyl)-2-naphthoic acid methyl ester
[0491] Step 3-1: NaBH was added to a solution of dimethyl naphthalene-2,7-dicarboxylate (100 g) in THF (1.60 L) under a nitrogen atmosphere 4 (30.9 g), then heated to 60°C. MeOH was added dropwise, heated to reflux for 6 hours, and further stirred at room temperature for 12 hours. Under ice-cooling, concentrated hydrochloric acid (70.0 mL) was added dropwise, stirred for 30 minutes, the resulting solid was filtered through celite, and the filtrate was concentrated under reduced pressure. To the residue was added EtOAc (2.00 L) and CHCl 3 (500 mL), and the resulting solid was filtered. with H 2 O washed the filtrate with MgSO 4 After drying, it was concentrated under reduced pressure. To the resulting residue was added CHCl 3 (1.30 L), and after stirring at room temperature for 12 hours, the solid was filtered. The filtrate was concentrated under reduced ...
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