In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 14452-30-3 as follows. name: 1-(3-Iodophenyl)ethanone
Ethyl 3-(3-iodophenyl)-3-oxopropanoate (0481) To a solution of diethyl carbonate (12.0 g, 101.6 mmol) in anhydrous toluene (100 mL) was added NaH (60% suspension in mineral oil, 3.25 g, 81.3 mmol) portionwise at 0 C under nitrogen atmosphere. After stirring at 0 C for 5 minutes, the mixture was warmed up to room temperature and l-(3-iodophenyl)ethanone (5.0 g, 20.3 mmol) was added dropwise over 10 minutes. The resulting mixture was heated at 110 C for 16 hours. The reaction was cooled to 0 C and quenched with CH3COOH (10 mL). H20 (50 mL) was added and the mixture was extracted with EtOAc (100 mL x 2). The combined organic layers were washed with saturated aqueous NaHC03 (100 mL), dried over anhydrous Na2S04, filtered and concentrated. The residue was purified by flash column chromatography on silical gel (0- 5 % EtOAc/PE) to afford the desired product as a red oil (4.0 g, 62% yield). 1H NMR (400 MHz, CDC13) delta 8.28 (s, 1H), 7.92 (d, / = 8.8 Hz, 1H), 7.90 (d, / = 8.0 Hz, 1H), 7.25-7.21 (m, 1H), 4.22 (q, / = 7.2 Hz, 2H), 3.95 (s, 1H), 1.27 (t, / = 7.2 Hz, 3H). LCMS (ESI): m/z 318.8 [M+H]+, RT = 0.93 min (LCMS Method E).
According to the analysis of related databases, 14452-30-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; GENENTECH, INC.; CONSTELLATION PHARMACEUTICALS, INC.; ALBRECHT, Brian K.; GEHLING, Victor S.; HARMANGE, Jean-Christophe; LAI, Tommy; LIANG, Jun; DRAGOVICH, Peter; ORTWINE, Dan; LABADIE, Sharada; ZHANG, Birong; KIEFER, Jim; WO2015/135094; (2015); A1;,
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