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. 823-57-4, name is 2-Bromo-5-chloroaniline, A new synthetic method of this compound is introduced below., Recommanded Product: 823-57-4
General procedure: To a solution of 2-bromoaniline (1.0 equiv.) and N,N-diisopropylethylamine (2.4 equiv.) in toluene was added cis-1,4-dichlorobut-2-ene (1.8 equiv.). The mixture was stirred at reflux until complete consumption monitored by TLC. The reaction was cooled to room temperature, diluted with water, and extracted with EtOAc. The combined organic layers were washed with saturated NaCl solution and dried over Na 2 SO 4 . The solvents were removed under reduced pressure, purified by flash chromatography to give the pure or crude desired product 3. The product 3 was dissolved in anhydrous THF, then was cooled to -78 oC, n-BuLi (1.2 equiv., 2.5 mol/L in n-hexane) was added dropwise to the mixture and keep temperature no more than -50 oC, the mixture was stirred for 30 minutes, (COOR3) 2 (1.0-1.2 equiv.) in THF was added dropwise at -78 oC and stirred at -78 oC for 2 h. The reaction was warmed to room temperature slowly, then quenched with saturated NH 4 Cl solution, and extracted with EtOAc. The combined organic layers were washed with saturated NaCl solution and dried over Na 2 SO 4 . The solvents were removed under reduced pressure, purified by flash chromatography to give the desired product 1.
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:
Article; Du, Hong-Jin; Lin, Chao; Wen, Xiaoan; Xu, Qing-Long; Tetrahedron; vol. 74; 52; (2018); p. 7480 – 7484;,
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