Synthesis
The general procedure for the synthesis of 2-bromo-1-(2-pyridyl)-1-acetone hydrobromide from 2-acetylpyridine was as follows: bromine (1.52 mL, 9.72 mmol) was slowly added dropwise to a 30% hydrobromide/acetic acid (12 mL) solution containing 2-acetylpyridine (3 g, 24.8 mmol) at 15 °C. After the dropwise addition was completed, the reaction mixture was warmed to 40 °C and kept stirring for 1 h. Subsequently, it was continued to be warmed to 75 °C and stirred for 1 h. The reaction mixture was then heated up to 40 °C and kept stirring for 1 h. Upon completion of the reaction, the reaction solution was cooled to 20 °C, ether (30 mL) was added and stirred at this temperature for 30 minutes. The resulting yellow precipitate was collected by filtration, and the precipitate was washed with ether (10 mL) and dried to afford the target product 2-bromo-1-(2-pyridyl)-1-acetone hydrobromide (6.81 g, 97.8% yield).
References
[1] Patent: CN105524056, 2016, A. Location in patent: Paragraph 0048; 0049; 0050
[2] Patent: WO2008/4117, 2008, A1. Location in patent: Page/Page column 85
[3] PLoS ONE, 2016, vol. 11, # 5,
[4] Patent: WO2017/17631, 2017, A2. Location in patent: Paragraph 00330
[5] Journal of Medicinal Chemistry, 2010, vol. 53, # 2, p. 787 - 797
