1228779-96-1, 3-Nitro-4-(((tetrahydro-2H-pyran-4-yl)methyl)amino)benzenesulfonamide is a Tetrahydropyrans compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
Into a 8-mL round-bottom flask, was placed a solution of 4-(4-[[2-(4-chlorophenyl)- 4,4-dimethylcyclohex-l-en-l-yl]methyl]piperazin- l-yl)-2-[l3-oxa-2,4,l0- triazatricyclo[7.4.0.0A[3,7]]trideca-l,3(7),5,8-tetraen-l0-yl]benzoic acid (35 mg, 0.06 mmol, 1.00 equiv) in dichloromethane (5 mL), 4-dimethylaminopyridine (27.8 mg, 0.23 mmol, 4.00 equiv), 3-nitro-4-[(oxan-4-ylmethyl)amino]benzene-l-sulfonamide (21.7 mg, 0.07 mmol, 1.20 equiv), EDCI (22 mg, 0.11 mmol, 2.00 equiv). The resulting solution was stirred for overnight at room temperature. The resulting mixture was concentrated under vacuum. The crude product was purified by Prep-HPLC with the following conditions (Waters-2767): Column, X-bridge RP18, 5um, l9* l00mm; mobile phase, 0.03% ammonia in water (0.03% NH4HC03 & NH40H ) and CH3CN (32% CH3CN up to 52% in 6 min); Detector, UV 254 nm. This resulted in 28.3 mg (54%) of 4-(4-[[2-(4-chlorophenyl)-4,4-dimethylcyclohex-l-en- l-yl]methyl]piperazin-l-yl)-N-([3-nitro-4-[(oxan-4-ylmethyl)amino]benzene]sulfonyl)-2-[l3- oxa-2,4,l0-triazatricyclo[7.4.0.0A[3,7]]trideca-l,3(7),5,8-tetraen-l0-yl]benzamide as a yellow solid. LC-MS-: (ES, m/z ): (ES, m/z): M+l=909, R.T= 1.52 min. The measurements of the retention were done with a reversed phase column (C18). Shimadzu LCMS 2020; 50*3.0 Kinetex 2.6u XB-C18 , 2.6 microm; Eluent A: water (0.05 % TFA); Eluent B: Acetonitrile; linear gradient. H-NMR: (CDCl3, 300 MHz) d: 8.70 (s, 1H), 8.46 (m, 2 H), 8.10-8.06 (m, 1 H), 7.89-7.60 (m, 1 H), 7.10 (s, 1 H), 6.94-6.71 (m, 5 H), 6.49 (s, 1 H), 6.16 (s, 1 H), 4.70- 4.65 (m, 2 H), 4.00-4.10 (m, 2 H), 3.67-3. l9(m, 7 H), 3.20-3.00(m, 4 H), 2.78(s, 1 H), 2.58- 2.52(m, 2 H), 2.27-2. l7(m, 3 H), 2.05-l.98(m, 4 H), 1.74-1.70 (m, 3 H), 1.55-1.40 (m, 3H), 0.98 (s, 6H).The measurements of the NMR spectra were done with BrukerAvancelll HD 300MHzwith a probe head of BBOF
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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