Benzimidazole 5-sulfonamide derivatives as cannabinoid 1 (CB1) receptor ligands
A halogen, compound technology, applied in the field of therapeutic compounds, can solve the problems of psychobehavioral side effects, abuse potential drug dependence and tolerance, etc.
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Embodiment 1
[0163] 2-tert-butyl-N, N-diethyl-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazole-5-sulfonamide
[0164]
[0165] Step A: 2-tert-Butyl-N,N-diethyl-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazole-5-sulfonamide
[0166]
[0167] 2-tert-Butyl-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazole-5-sulfonyl chloride (61.2 mg, 0.165 mmol) (for preparation see Step B below , C, D, E, F, G and H) were added to a solution of diethylamine (0.2 mL, 1.93 mmol) and DMAP (50 mg, 0.41 mmol) in MeCN (5 mL). The reaction mixture was stirred overnight at room temperature, diluted with ethyl acetate (60 mL), washed with NH 4 Cl (2x5mL), NaCl (2x5mL) washed, and washed with Na 2 SO 4 dry. The crude product was purified by MPLC (silica gel, eluting with hexane / ethyl acetate (1:1)) to afford 20.5 mg (30%) of the title compound as a white solid. 1 H NMR (400MHz, methanol-D 4 )δ 1.13(t, J=7.13Hz, 6H), 1.46-1.63(m, 4H), 1.66(s, 9H), 2.25-2.48(m, 1H), 3.22-3.29(m, 4H), 3.31- 3.41(m, ...
Embodiment 2
[0190] 2-tert-butyl-5-(piperidin-1-ylsulfonyl)-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazole
[0191]
[0192] According to the same operation as in Example 1, step A, 2-tert-butyl-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazole-5-sulfonyl chloride (61 mg, 0.17 mmol), piperidine (0.2 mL, 2.0 mmol) and DMAP (50 mg, 0.41 mmol) in MeCN (5 mL). The crude product was purified by MPLC (silica gel, eluting with hexane / ethyl acetate (1:1)) to afford 31 mg (45%) of the title compound as a white solid. 1 H NMR (400MHz, methanol-D 4 )δ 1.40(m, 2H), 1.47-1.64(m, 8H), 1.65(s, 9H), 2.25-2.48(m, 1H), 2.92-3.05(m, 4H), 3.29-3.39(m, 2H ), 3.88-3.98(m, 2H), 4.50(d, J=7.62Hz, 2H), 7.82(dd, J=8.69, 1.66Hz, 1H), 8.01(d, J=8.79Hz, 1H), 8.06 (d, J=1.56Hz, 1H); MS(ESI)(M+H) + = 420.0; C 22 h 33 N 3 o 3 S+1.10 TFA+0.50 H 2 O+0.10CH 3 Theoretical for OH (557.23): C, 52.38; H, 6.42; N, 7.54; Found: C, 52.38; H, 6.43; N, 7.58.
Embodiment 3
[0194] 2-tert-butyl-5-(isoxazolidin-2-ylsulfonyl)-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazole
[0195]
[0196] According to the same operation as in Example 1, step A, 2-tert-butyl-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-benzimidazole-5-sulfonyl chloride (61 mg, 0.17 mmol), isoxazolidine hydrochloride (44 mg, 0.40 mmol), DIPEA (0.2 mL, 149 mg, 1.15 mmol) and DMAP (50 mg, 0.41 mmol) in MeCN (5 mL). The crude product was purified by MPLC (silica gel, eluting with hexane / ethyl acetate (1:1)) to afford 24 mg (36%) of the title compound as a white solid. 1 HNMR (400MHz, methanol-D 4 )δ 1.43-1.61(m, 4H), 1.63(s, 9H), 2.02-2.19(m, 2H), 2.25-2.42(m, 1H), 3.29-3.38(m, 2H), 3.64-3.73(m , 2H), 3.86(t, J=7.13Hz, 2H), 3.88-3.96(m, 2H), 4.49(d, J=7.42Hz, 2H), 7.98(d, J=1.56Hz, 1H), 7.99 (s, 1H), 8.24 (d, J=0.78Hz, 1H); MS (ESI) (M+H) + = 408.0; C 20 h 29 N 3 o 4 Calcd for S+1.20TFA+0.20 EtOAc (561.99): C, 49.58; H, 5.70; N, 7.48; Found: C, 49.74; H, 5.53; N, 7.46.
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