Synthetic Route of 133541-45-4, A common heterocyclic compound, 133541-45-4, name is 4-Bromo-2,5-difluorobenzonitrile, molecular formula is C7H2BrF2N, 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.
To a suspension of sodium hydride (4.04 g, 100 mmol, 60 % purity) in THF (25 mL) was added tert-butyl N-(2-hydroxypropyl)carbamate (8.84 g, 50.5 mmol) at 0 “C. The resulting mixture was stirred at 0 C for 0.5 h, then a solution of 4-bro mo-2,5-difluorobenzonitrile (10 g, 45.9 mmol) in THF (25 mL) was added. The mixture was stirred at 0 C for 0.5 h. The reaction mixture was diluted with water and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure to give a residue, which was purified by column chromatography (silica gel, petroleum ether/ethyl acetate = 50/1 to 10/1 ) to give the desired product (13 g, 34.8 mmol, 76% yleld) as a white solid.MS (M+H+): 397.11H NMR (400 MHz, CDCI3) delta [ppm]: 7.33-7.30 (t, J = 6Hz, 1 H), 7.27-7.24 (t, J = 6Hz, 1 H), 4.99 (s, 1 H), 4.57 (s, 1 H), 3.53-3.48 (m, 1 H), 3.33-3.28 (m, 1 H), 1 .62-1 .45 (q, 9H), 1.36-1.26 (m, 3H).
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.