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. 330793-38-9, name is 4-Bromo-2-methoxybenzonitrile, A new synthetic method of this compound is introduced below., name: 4-Bromo-2-methoxybenzonitrile
To a mixture of 4-bromo-2-methoxy benzonitrile (1 g, 4.72 mmol), butyl vinyl ether (2.362 g, 23.58 mmol), l,3-bis(diphenylphosphino)propane (0.097 g, 0.236 mmol), palladium (II) acetate (0.053 g, 0.236 mmol) and l-butyl-3-methylimidazolium tetrafluoro borate (0.533 g, 2.358 mmol) in DLC/MSO (4.72 ml) was added diisopropylamine (0.807 ml, 5.66 mmol) in a microwave vial. The reaction mixture was degassed with argon and stirred at 115°C for 18h. The mixture was partitioned between EtOAc and H20 and the aqueous layer was extracted with EtOAc (3x). The combined organic phase was washed with brine, dried over anhydrous MgS04, and filtered. The residue was then dissolved in MeOH/DLC/MSO (25ml/5ml), then 3N HC1 (20 ml) was added. The mixture was stirred at rt for 3h. After concentration the residue was partitioned between DCM and water and the aqueous layer was extracted with DCM (3x). The combined organic phase was washed with brine, dried over anhydrous MgS04, and filtered. The filtrate was concentrated and purified by silica gel column chromatography using (0-60)percentEtOAc/Hexanes as mobile phase to give the title product as a pale yellow solid.
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; MERCK SHARP & DOHME CORP.; CHOBANIAN, Harry; PIO, Barbara; GUO, Yan; DING, Fa-Xiang; DONG, Shuzhi; WALSH, Shawn, P.; JIANG, Jinlong; KIM, Dooseop; WO2015/95097; (2015); A2;,
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