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. 49834-22-2, name is 3-Bromo-N-methylbenzamide, A new synthetic method of this compound is introduced below., Recommanded Product: 3-Bromo-N-methylbenzamide
200 mg of tetrakistriphenylphosphine palladium was added under cooling with ice to a solution of 0.86 g of N-methyl-3-bromobenzamide in a mixed solvent of 10 ml of toluene and 3 ml of ethanol, followed by stirring for 20 minutes. 0.93 g of 4-chloro-2,6-dimethylbenzene boronic acid and 4.5 ml of a 2M sodium carbonate aqueous solution were added thereto, and the reaction system was flushed with nitrogen, followed by reflux under heating for 9 hours. After cooling, 50 ml of cold water was added, and then, 50 ml of ethyl acetate was added. The precipitate was filtered off. Then, the organic layer was separated from the filtrate. The water layer was extracted again with 50 ml of ethyl acetate. The organic layers were put together and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel (Silica gel 60N; spherical and neutral, manufactured by Kanto Kagaku) column chromatography (developing solvent of n- hexane: ethyl acetate=1 : 1) to obtain 0.40 g of the objective compound having a melting point of 137. 1C. Further, NMR of this compound was as follows. 1H-NMR 5 (ppm) 1.98 (s, 6H), 3.02 (d, 3H; J =5. 1 Hz), 6.18 (bs, lH), 7.10 (s, 2H), 7.24 (d, lH ; J =7. 5 Hz), 7.49 (t, lH; J =7. 5 Hz), 7.51 (s, lH), 7.75 (d, lH; J =7. 5 Hz)
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; ISHIHARA SANGYO KAISHA, LTD.?; WO2005/44007; (2005); A1;,
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