Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 261762-56-5, name is 1-Chloro-2-fluoro-3-methoxybenzene, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H6ClFO
To a 0 C solution of 1-chloro-2-fluoro-3-methoxybenzene (1.606 g, 10 mmol) in acetic acid (5.00 ml) was added fuming nitric acid (0.93 3 ml, 20.00 mmol) followed bythe dropwise addition of sulfuric acid (2.132 ml, 40.0 mmol). After 30 mm, the reaction mixture was poured into water and diluted with ethyl acetate. The organic phase was separated and washed 2x with saturated NaHCO3 followed by a final brine wash. The organic solution was then dried over Mg504, filtered, concentrated and purify by ISCO (120g, 10-50% EtOAc/Hexanes, 25 mm. Desired regioisomer eluted second) affordingIntermediate I-43A (1.lOg, 5.35 mmol, 53% yield) as a yellow solid. LC-MS: Method H,RT = 1.13 mm, MS (ESI) m/z: No Ionization Observed (M+H)t ?H NMR (400MHz, CHLOROFORM-d) oe 7.89 (dd, J=9.2, 2.2 Hz, 1H), 6.95 (dd, J=9.4, 7.6 Hz, 1H), 4.00 (s, 3H). Regiochemistry confirmed through NMR analysis of both regioisomeric products.
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.
Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; ZHANG, Xiaojun; PRIESTLEY, Eldon Scott; BATES, J. Alex; HALPERN, Oz Scott; REZNIK, Samuel Kaye; RICHTER, Jeremy M.; (1137 pag.)WO2018/13774; (2018); A1;,
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