Compounds and compositions for treating conditions associated with nlrp activity
A compound, the technology of -Z-Q, applied in the treatment of a kind of anti-TNFα resistance, the pathology and/or symptoms and/or fields of the disease, disease or disorder, can solve the low permeability, poor systemic biological Utilization etc.
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[1930] Racemic compounds of the present invention can be resolved into the individual enantiomers using a variety of known methods. For example, chiral stationary phases may be used, and elution conditions may include normal phase or supercritical fluids with or without acidic or basic additives. Enantiomerically pure acids or bases can be used to form diastereomeric salts with racemic compounds so that the pure enantiomers can be obtained by fractional crystallization. Racemates may also be derivatized with enantiomerically pure auxiliary reagents to form diastereomeric mixtures which may be separated. The auxiliary is then removed to give the pure enantiomer.
[1931] The following abbreviations have assigned meanings:
[1932] ACN = acetonitrile
[1933] BTC = trichloromethyl chloroformate
[1934] Boc = tert-butoxycarbonyl
[1935] Davephos=2-dicyclohexylphosphino-2'-(N,N-dimethylamino)biphenyl
[1936] DCM = dichloromethane
[1937] DEA = Diethylamine
[1938] DMF...
example 1-3
[2160]
[2161] Step 1: N'-((1,2,3,5,6,7-hexahydro-symmetricindacene-4-yl)carbamoyl)-N,N-dimethylmethane-sulfonimide Amide
[2162] Into a 50 mL round bottom flask purged and maintained with a nitrogen inert atmosphere was placed N,N-dimethylmethanesulfonylimide amide (220 mg, 1.8 mmol, 1.0 equiv) and TEA (0.75 mL, 5.4 mmol, 3.0 equiv ) in THF (15.0 mL). To the solution was added 4-isocyanato-1,2,3,5,6,7-hexahydro-symmetric indacene (286 mg, 1.4 mmol, 0.8 equiv). The solution was stirred overnight at ambient temperature. The reaction mixture was concentrated under reduced pressure, and the residue was purified by preparative HPLC with the following conditions: Column: XBridge Prep OBD C18 column, 30×150mm, 5um; Mobile phase A: water (10mmol / L NH 4 HCO 3 +0.1% NH 4 OH), mobile phase B: ACN; flow rate: 60 mL / min; gradient: 30% B to 50% B in 7 min; detector, UV 220 / 254 nm. This yielded 80 mg of N'-((1,2,3,5,6,7-hexahydro-symmetricindacen-4-yl)carbamoyl)-N,N-dimethylmetha...
example 10-12
[2171]
[2172] Step 1: N-(tert-butyldiphenylsilyl)-3-(dimethylamino)-N'-((1,2,3,5,6,7-hexahydro-symmetric indacene -4-yl)carbamoyl)propane-1-sulfonylimide amide
[2173] Put N-(tert-butyldiphenylsilyl)-3-(dimethylamino)propane-1-sulfonylimide amide (300mg , 0.7 mmol, 1.0 equiv) and NaH (60% wt in mineral oil, 44 mg, 1.1 mmol, 1.5 equiv) in THF (10 mL). To the solution was added 4-isocyanato-1,2,3,5,6,7-hexahydro-symmetric indacene (148 mg, 0.7 mmol, 1.0 equiv) at 0°C. The resulting solution was stirred for another 1 h at 0 °C in a water / ice bath, then quenched by addition of water. The reaction mixture was extracted with ethyl acetate, and the combined organic layers were concentrated to give 300 mg of N-(tert-butyldiphenylsilyl)-3-(dimethylamino)-N '-((1,2,3,5,6,7-hexahydro-symmetricindacen-4-yl)carbamoyl)propane-1-sulfonylimide amide. MS-ESI: 602.9 (M+1).
[2174] Step 2: 3-(Dimethylamino)-N'-((1,2,3,5,6,7-hexahydro-symmetricindacene-4-yl)carbamoyl)propane-1-sulfo ...
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