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 24468-88-0 as follows. HPLC of Formula: C11H15Br2N
To a solution of compound 1-2 (2.56 g, 14.34 mmol) and compound 32-1 (6.905 g, 21.51 mmol) in DMF (15 mL) under N2 was added NaH (1.434g, 35.85 mmol, 60% dispersed in Mineral oil). The mixture was stirred at 50 C for 18 hours, cooled to rt, and quenched with water (20 mL). The mixture was extracted with EtOAc (150 mL x 3). The combined organic phases were washed with water, dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (hexane/EtOAc (v/v) = 8/1) to give the title compound 32-2 (0.752 g, 14.9%). The compound was characterized by the following spectroscopic data: MS-ESI: m/z 352.1 [M+H]+; and1H NMR (400 MHz, CDCl3): delta 7.63-7.56 (m, 1H), 7.41-7.22 (m, 6H), 3.82 (d, 6H), 3.56 (s, 2H), 3.03 (s, 2H), 2.98-2.89 (m, 2H), 2.24-2.00 (m, 4H), 1.37 (d, J = 11.8 Hz, 2H).
According to the analysis of related databases, 24468-88-0, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Sunshine Lake Pharma Co., Ltd.; ZHANG, Jiancun; ZHANG, Yingjun; XIE, Hongming; REN, Qingyun; LUO, Huichao; YU, Tianzhu; TAN, Yumei; EP2730572; (2015); B1;,
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