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
A 50-L jacketed reactor equipped with a mechanical stirrer, nitrogen inlet/outlet, heating mantle and reflux condenser was inerted with flow through nitrogen and charged with 3-nitro-4-(((tetrahydro-2H-pyran-4-yl)methyl)amino)benzenesulfonamide (493 g, 0.95 equiv) EDCI (552 g, 1.75 equiv), DMAP (402 g, 2. equiv) and DCM (5 L, 5 vo I). Separately a 20-L carboy was charged with 2-((1 /-/-Pyrrolo[2,3-b]pyridin-5-yl)oxy)- 4-(4-((4′-chloro-5,5-dimethyl-3,4,5,6-tetrahydro-[1 ,T-biphenyl]-2-yl)methyl)piperazin-1- yl)benzoic acid hydrochloride salt (1 kg, 1.64 moles), DCM (10 L, 10 vol) and stirred. Triethylamine (920 mL, 4.00 equiv.) was added and the batch was stirred at room temperature. This solution was dosed into the jacketed reactor over 3 h. The batch was stirred at room temperature for 8-25 h indicated reaction was complete. Batch was distilled down to ~ 5 L and diluted with 2-MeTHF (15 L, 15 vol). The batch was then distilled from ~ 20 L to ~10 L. b) Work up: The batch temperature was adjusted to 40C over 15 min and was washed with two 10% AcOH washes (10 L each) and then separating phases. The batch was then washed with 2 N NaOH (10 L, 10 vol) by heating to 40 ¡À 5 C after addition, stirring for 15 min and then phase separation. Isopropyl alcohol (IPA, 15 L, 15 vol) was charged to the reactor and the batch was distilled down from 21 L to ~ 10 L. Separately maleic acid (287 g, 1.5 equiv) was dissolved in water (1 L, 1 vol) and this solution was charged to the reactor. Upon addition of the maleic acid solution, it was heated to 70 C over 20 min and aged. The slurry was then filtered and rinsed with IPA (2.0 L). The cake was dried to constant weight to give crude maleate salt (1.525 kg)., 1228779-96-1
1228779-96-1 3-Nitro-4-(((tetrahydro-2H-pyran-4-yl)methyl)amino)benzenesulfonamide 57474953, aTetrahydropyrans compound, is more and more widely used in various fields.
Reference£º
Patent; ALBANY MOLECULAR RESEARCH, INC.; GREGG, Brian, Thomas; GEISS, William, Bert; HERR, Robert, Jason; RAI, Ravi, R; (39 pag.)WO2020/23435; (2020); A1;,
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