Electric Literature of 330793-38-9, These common heterocyclic compound, 330793-38-9, name is 4-Bromo-2-methoxybenzonitrile, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
A mixture of 4-bromo-2-methoxybenzonitrile (3.0 g, 14 mmol) , Boc2O (3.24 g, 15.6 mmol) , and Raney Ni (10, 0.6 g) in EtOAc (100 mL) was heated under 40 psi H2atmosphere at 70 for 36 h. The product mixture was filtered, and the filtrate concentrated. The residue was purified by silica gel chromatography eluting with EA: PE 1:30 to 1:10 to afford the title compound.1H NMR (400 MHz, CDCl3) delta 7.09-7.18 (m, 1H) , 7.01 -7.08 (m, 1H) , 6.98 (s, 1H) , 4.23 (d, J 5.8 Hz, 2H) , 3.83 (s, 3H) , 1.44 (s, 9H) . MS : m/z 259 (M – 56) .
The synthetic route of 330793-38-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MERCK SHARP & DOHME CORP.; COOKE, Andrew J.; PITTS, Daniel; JOHNSON, Adam; BESHORE, Douglas C.; HURZY, Danielle; MITCHELL, Helen; FRALEY, Mark; MCCOMAS, Casey; SCHIRRIPA, Kathy; MERCER, Swati P.; NANDA, Kausik; MENG, Dongfang; WU, Jane; BABAOGLU, Kerim; LI, Chun Sing; MAO, Qinghua; QI, Zhiqi; (156 pag.)WO2016/54807; (2016); A1;,
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