Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 13421-13-1, name is 4-Chloro-2-iodobenzoic acid, A new synthetic method of this compound is introduced below., Application In Synthesis of 4-Chloro-2-iodobenzoic acid
To a solution of 4-chloro-2-iodobenzoic acid (1-1, X?I) (CAS :13421-13-1; Aldrich, SKU: 560146) (3 g, 10.62 mmol) and N,O-dimethylhydroxylamine hydrochloride (CAS : 6638-79-5; Sigma Aldrich, SKU: D163708) (1.2 g, 12.31 mmol) in dimethylformamide (DMF) (30 mL), was added dropwise triethyl amine (TEA) (7.4 mL, 53.14 mmol), followed by the addition of (1-[bis(dimethylamino)methylene]-1H-1,2,3-triazolo[4,5-b]pyridinium 3-oxid hexafluorophosphate) (HATU) (6.1 g, 16.05 mmol). The reaction mixture was stirred at RT for 16 h and then diluted with CH2Cl2 and H2O, and the aqueous layer was extracted with CH2Cl2 (4×20 mL). The combined organic layers were washed with brine, dried over Na2SO4, filtered, concentrated in vacuo and purified by silica gel chromatography (ethyl acetate/hexanes 1:4) to afford the title compound as a white solid (3.2 g. LCMS (MH+): 325.9. 1H NMR (400 MHz, CDCl3-d): delta 3.11-3.38 (m, 3H), 3.47-3.90 (m, 3H), 7.20 (d, J=8 Hz,1H), 7.37 (d, J=2 Hz, 1H), 7.84 (s,1H).
The synthetic route of 13421-13-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Karos Pharmaceuticals, Inc.; De Lombaert, Stephane; Goldberg, Daniel R.; (12 pag.)US2016/257633; (2016); A1;,
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