As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 76176-87-9, name is Thiomorpholine-1-oxide hydrochloride. This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 76176-87-9
To the stirred solution of [cis-3-(4-amino-5-iodo-pyrrolo [2,3-d]pyrimidin-7-yl)-cyclobutyl] methanol (Intermediate M: 348 mg, 1.0 mmol) and acetonitrile (70 mL) was added IBX (Atlantic SciTech 86900: 561 mg, 2.0 mmol, 2 eq). The reaction mixture was stirred for 1 h at 80 C. Th e reaction mixture was filtered at 40 C and the filtrate was concentrated. To the residue was added subsequently DCM (50 ml_), ethyl-diisopropyl-amine (3.43 ml_, 20 mmol, 20 eq), 1-oxide thiomorpholin hydrochloride (312 mg, 2.0 mmol, 2 eq) and sodium triacetoxyborohy- dride (637 mg, 3.0 mmol, 3 eq) with stirring at rt. The reaction mixture was stirred for 1 h at rt and then partitioned between NaHC03 1M and EtOAc. The combined organic layers were washed with water and brine, dried (Na2S04), filtered and concentrated. The residue was purified by silica gel column chromatography (DCM/MeOH/NH3aq, 200:20:1) to afford 238 mg of the title compound as pale yellow crystals: HPLC-MS: M+H = 446.2 (Rt = 0.41) (Method X); TLC; Rf = 0.26 (DCM/MeOH/NH3aq, 200:20: 1).
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Reference£º
Patent; NOVARTIS AG; IRM LLC; CHEN, Bei; FAIRHURST, Robin, Alec; FLOERSHEIMER, Andreas; FURET, Pascal; GUAGNANO, Vito; JIANG, Songchun; LU, Wenshuo; MARSILJE, Thomas, H.; MCCARTHY, Clive; MICHELLYS, Pierre-Yves; STAUFFER, Frederic; STUTZ, Stefan; VAUPEL, Andrea; WO2011/29915; (2011); A1;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem