The synthetic route of 1228779-96-1 has been constantly updated, and we look forward to future research findings.
With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1228779-96-1,3-Nitro-4-(((tetrahydro-2H-pyran-4-yl)methyl)amino)benzenesulfonamide,as a common compound, the synthetic route is as follows.
Into a 40-mL round-bottom flask, was placed 4-(4-((4?-chloro-5, 5-dimethyl-3, 4, 5, 6-tetrahydro-[l, 1?-biphenyl] -2-yl)methyl)piperazin-l-yl)- 2-(3-methoxy-3,4-dihydro-2H-pyrrolo[3?,2?:5,6]pyrido[2,3-b][l,4]oxazepin-l(7H)- yl)benzoic acid (50 mg, 0.08 mmol, 1 equiv), DCM (3 mL), 3-nitro-4-[[(oxan-4- yl)methyl]amino]benzene-l-sulfonamide (25.2 mg, 0.08 mmol, 1.00 equiv), EDCI (30.6 mg, 0.16 mmol, 2 equiv), DMAP (39.0 mg, 0.32 mmol, 4 equiv). The resulting solution was stirred for overnight at 25 degrees C. The resulting mixture was concentrated under vacuum. The residue was applied onto a silica gel column with dichloro methane/methanol (10: 1). The crude product was purified by Flash- Prep-HPLC with the following conditions (IntelFlash-l): Column, C18 reversed phase column; mobile phase, Water (10MMOF/F NH4HC03+0.05%NH3.H20) and CH3CN (20.0% CH3CN up to 90.0% in 30 min); Detector, UV 220 nm. This resulted in 32 mg (40.0%) of 4-(4-((4?-chloro-5,5-dimethyl-3, 4,5,6- tetrahydro- [1,1? -biphenyl] -2-yl)methyl)piperazin- 1 -yl) -2-(3 -methoxy-3 ,4-dihydro-2H- pyrrolo[3?,2?:5,6]pyrido[2,3-b][l,4]oxazepin-l(7H)-yl)-N-((3-nitro-4-(((tetrahydro-2H- pyran-4-yl)methyl)amino)phenyl)sulfonyl)benzamide as a yellow solid. FC-MS: (ES, m/z): M+l=953, R,T= 3.44 min. 1H NMR (300 MHz, DMSO-d6, ppm) d 11.00 (ds, 1H), 8.56 (s, 2H), 7.47-7.44 (m, 2H), 7.36-7.33 (m, 2H), 7.08-7.04 (m, 3H), 6.78-6..65 (m, 2H), 6.57-6.54 (m, 1H), 6.43 (s, 1H), 6.04 (s, 1H), 4.05-3.15 (m, 20H), 3.13 (s, 1H), 2.70-2.35 (m, 4H), 2.03 (s, 3H), 1.92-1.90 (m, 1H), 1.89-1.87 (m, 2H), 1.71-1.67 (m, 2H), 1.53-1.45 (m, 3H), 0.97 (s, 6H, 1228779-96-1
The synthetic route of 1228779-96-1 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; NEWAVE PHARMACEUTICAL INC.; CHEN, Yi; (475 pag.)WO2020/41406; (2020); A1;,
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