The synthetic route of 96568-04-6 has been constantly updated, and we look forward to future research findings.
Application of 96568-04-6 , The common heterocyclic compound, 96568-04-6, name is Ethyl 3-(2,6-Dichloro-5-fluoro-3-pyridyl)-3-oxopropionate, molecular formula is C10H8Cl2FNO3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
General procedure: 4.1.4.1. 5-(2,6-Dichloro-5-fluoropyridin-3-yl)-3-phenyl-2-(trifluoromethyl)pyrazolo[1,5-a]pyrimidin-7(4H)-one (17)A solution of intermediate 5a (0.227 g, 1 mmol) and ethyl 3-(2,6-dichloro-5-fluoropyridin-3-yl)-3-oxopropanoate (0.28 g, 1 mmol) in acetic acid (8 ml) was added to a teat glass (40 ml) of Syncore Reactor, keeping the temperature at 125 C and the rotational speed of the device at 300 rpm for 4 h. After this period, the solvent of reaction was concentrated to half under reduced pressure by Syncore Polyvap, and cooled to about 15 C gradually. The mixture was filtered and the solid was washed with acetic acid and water to pH 7, to obtain the compound 17 (0.35 g, Yield: 80%, Purity: 98% by HPLC-DAD) as a white floccular solid. mp >300 C; ESI-Ms (m/z): 443.2 [M + H]+; 1H NMR (500 MHz, DMSO-d6) delta: 7.52 (m, 3H, Ph-H), 7.47 (m, 2H, Ph-H), 6.17 (s, 1H, 6-CH), 8.41 (d, 1H, J = 8, pyridine 4-CH), 12.90 (brs, 1H, NH); 13C NMR (125 MHz, DMSO-d6) delta: 99.33 (6-CH), 104.56 (3-C), 155.63 (7-CO), 152.57, 154.63 (5-C), 140.75 (2-C), 130.65 (Ph-C), 129.22 (Ph-C), 128.89 (Ph-C), 127.94 (Ph-C), 122.86 (CF3), 146.91 (pyridine-C), 142.59 (pyridine-C), 137.94 (pyridine-C), 130.44 (pyridine-C), 130.26 (pyridine-C); HRMS (ESI) calcd for C18H9Cl2F4N4O ([M + H]+), 443.0090; found 443.0085; IRvmax (KBr):1701 (CO), 1629, 1558, cm-1.
The synthetic route of 96568-04-6 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Qi, Jinlong; Zhang, Fan; Mi, Yi; Fu, Yan; Xu, Wen; Zhang, Diqun; Wu, Yibing; Du, Xiaona; Jia, Qingzhong; Wang, Kewei; Zhang, Hailin; European Journal of Medicinal Chemistry; vol. 46; 3; (2011); p. 934 – 943;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem