Electric Literature of 930-62-1, 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 930-62-1 as follows.
A mixture of 2,4-dimethyl-lH-imidazole (5.00 g, 52.0 mmol),1 ,2-difluoro-4~nitrobenzene (8.27 g, 52.0 mmol), and sodium bicarbonate (4.37 g, 52.0 mmol) in DMSO (100 mL) was heated at 80 0C for 24 h . The reaction mixture was allowed to cool to rt and was poured into water (800 mL). The aqueous mixture was extracted with EtOAc (3 x 200 mL). The combined organic extracts were sequentially washed with water (500 mL) and brine solution (100 mL). The organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo. The dark residue was dissolved in ethyl acetate (200 mL). Hexane (50 mL) was added to the solution. The resulting mixture was allowed to age for 72 h at it. The resulting solid was collected by vacuum filtration. The solid was dried under high vacuum to afford l-(2-fluoro-4-nitrophenyl)-2,4-dimethyl-lH-imidazole (6.68 g, 27.8 mmol., 54 % yield) as a yellow crystalline solid. LC-MS (M+H)+ = 236.1. IH NMR (500 MHz, CHLOROFORM-d) B ppm 8.13 – 8.22 (m, 2 H), 7.51 (dd, J=8.9, 7.3 Hz, 1 H), 6.72 (s, 1 H), 2.28 – 2.36 (m, 3 H), 2.22 – 2.28 (m, 3 H).
According to the analysis of related databases, 930-62-1, the application of this compound in the production field has become more and more popular.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; MARCIN, Lawrence, R.; THOMPSON, Lorin, A., III; BOY, Kenneth, M.; GUERNON, Jason, M.; HIGGINS, Mendi, A.; SHI, Jianliang; WU, Yong-Jin; ZHANG, Yunhui; MACOR, John, E.; WO2010/83141; (2010); A1;,
Imidazole – Wikipedia,
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