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 1252046-13-1 as follows. COA of Formula: C7H3BrIN
Add bromo-(2-ethoxy-2-oxo-ethyl)zinc (2.97 g, 12.7 mmol) (prepared according to Example 9A) to a mixture of 2-bromo-5-iodo-benzonitrile (2.60 g, 8.44 mmol), bis(dibenzylideneacetone)palladium (0.121 g, 0.211 mmol) and 4,5-bis(diphenylphosphino )5 9,9-dimethylxanthene (0.122 g, 0.211 mmol) in THF (20 mL), then the reaction mixture is stirred at 65 C for 1 h under nitrogen. The reaction mixture is quenched with water (10 mL). The result mixture is extracted with EtOAc (10 mL x 3). The combined organic phases are washed with water (1 0 mL ), concentrated to afford a black residue, which is purified by column chromatography on silica gel eluting with PE:EtOAc (20: 1) to afford the title 10 compound (1.00 g, 42.0% Yield) as a yellow solid. 1H NMR (400MHz, CD3Cl) 8 = 7.65 (d, J = 8.4 Hz, 1H), 7.60 (d, J = 2.0 Hz, 1H), 7.39 (dd, J = 2.0, 8.4 Hz, 1H), 4.18 (q, J = 7.2 Hz, 2H), 3.61 (s, 2H), 1.28 (t, J = 7.2 Hz, 3H)
According to the analysis of related databases, 1252046-13-1, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ELI LILLY AND COMPANY; LILLY CHINA RESEARCH AND DEVELOPMENT CO., LTD.; MA, Tianwei; WU, Liang; ZHANG, Xuejun; (109 pag.)WO2019/41340; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com