03/9/2021 News Extracurricular laboratory: Synthetic route of 100367-39-3

At the same time, in my other blogs, there are other synthetic methods of this type of compound,100367-39-3, 4-Bromo-2-methoxypyridine, and friends who are interested can also refer to it.

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.100367-39-3, name is 4-Bromo-2-methoxypyridine, molecular formula is C6H6BrNO, molecular weight is 188.0219, as common compound, the synthetic route is as follows.Recommanded Product: 4-Bromo-2-methoxypyridine

To a resealable reaction pressure vessel under nitrogen was added 1.0 equiv of 55 (266 mg, 0.665 mmol), Pd(PPh3)4 (38 mg, 0.033 mmol, 5 mol %), K2C03 (184 mg, 1.33 mmol, 2.0 equiv), 2-methoxy-4-bromopyridine (137 mg, 0.732 mmol, 1.1 equiv), dioxane (20 mL) and water (2 mL). The mixture was degassed through bubbling nitrogen for 40 min and heated at 110 C overnight. After cooling to room temperature, water (20 mL) was added and the organic product was extracted using EtOAc (3 x 30 mL). The combined organic layers were dried over MgS04, filtered through Celite and the solvent removed in vacuo. The residual was purified by flash chromatography to provide 160 mg (63%) of 58 as colorless oil. 1H NMR (300 MHz, CDC13) delta 1.42 (br s, 9H), 1.49-1.63 (m, 2H), 1.86-1.98 (m, 3H), 2.00-2.07 (m, 1H), 2.96-3.01 (m, 1H), 3.92 (s, 3H), 4.30 (s, 1H), 4.42 (br s, 1H), 6.81 (dd, J = 5.7, 2.4 Hz, 1H), 7.25 (d, J= 2.2 Hz, 1H), 8.22 (t, J= 1.9 Hz, 1H), 8.53 (d, J= 5.7 Hz, 1H), 8.56 (d, J= 2.0 Hz, 1H), 9.00 (d, J = 2.0 Hz, 1H); 13C NMR (CDC13) delta 28.3 (3 C), 28.8, 29.9, 40.2, 45.8, 55.9, 61.8, 79.7, 107.2, 108.6, 132.9, 134.7, 140.9, 146.2, 149.1, 151.1, 155.0, 156.7 166.5; MS (ESI) m/z 382.7 (M+H)+.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,100367-39-3, 4-Bromo-2-methoxypyridine, and friends who are interested can also refer to it.

Reference:
Patent; RESEARCH TRIANGLE INSTITUTE; CARROLL, Frank Ivy; ONDACHI, Pauline Wanjiku; WO2012/24615; (2012); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem