Synthesis
General procedure for the synthesis of 5-bromo-2-methylpyrimidine from 2-methyl-5-bromopyrimidine-4-carboxylic acid: 5-bromo-2-methylpyrimidine-4-carboxylic acid (350 mg, 1.6 mmol) was dissolved in xylene (5 mL), and the reaction was carried out at reflux for 2 hours. After the reaction was completed, the reaction mixture was cooled to room temperature and directly sampled onto a silica gel column. Gradient elution with petroleum ether and petroleum ether solution containing 5% (v/v) ethyl acetate was carried out sequentially, and the target fraction was collected to give 5-bromo-2-methylpyrimidine (170 mg, 61% yield) as a white solid.LC-MS (m/z): 173 [M + H]+. 1H NMR (400 MHz, DMSO-d6) δ: 2.59 (s, 3H), 8.87 ( s, 2H).
References
[1] Patent: WO2011/130628, 2011, A1. Location in patent: Page/Page column 176
[2] Patent: US2013/102595, 2013, A1. Location in patent: Paragraph 0366
[3] Patent: JP2015/187145, 2015, A. Location in patent: Paragraph 0320
[4] Patent: WO2014/131855, 2014, A1. Location in patent: Page/Page column 56
[5] Collection of Czechoslovak Chemical Communications, 1949, vol. 14, p. 223,228
