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. 39478-78-9, name is 5-Bromo-2-methylaniline, A new synthetic method of this compound is introduced below., Quality Control of 5-Bromo-2-methylaniline
N-(5-bromo-2-methylphenyl)acrylamide (1): To a solution of 5-bromo-2- methylaniline (2.0 g, 10.8 mmol) in dichloromethane (10 mL), diisopropylethylamine (4.18 g, 32.3 mmol) and acryloyl chloride (1.16 g, 12.8 mmol) were added at -78C. The resulting mixture was stirred at room temperature for 30 min. After completion of reaction, the reaction mixture was quenched with water and the aqueous solution was extracted with dichloromethane (2×40.0 mL). The organic layer was washed with water followed by brine solution. The organic layer was dried over anhydrous sodium sulfate and concentrated over reduced pressure. The residue was triturated with n-pentane to afford 1 (2.2 g, 85%) as an off white solid. 1H NMR (400 MHz, CDCls) delta 2.23 (s, 3H), 5.79-5.82 (dd, J = 1.1, 10.2 Hz, 1H), 6.23-6.30 (dd, J = 10.2, 16.8 Hz, 1H), 6.42 (dd, J = 1.1, 16.8 Hz, 1H), 6.99 (brs, 1H), 7.04 (d, J = 8.1 Hz, 1H), 7.20 (m, 1H), 8.20 (brs, 1H). MS m/z (M-H): 238.0
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; CELGENE AVILOMICS RESEARCH, INC.; ALEXANDER, Matthew David; MCDONALD, Joseph John; NI, Yike; NIU, Deqiang; PETTER, Russell C.; QIAO, Lixin; SINGH, Juswinder; WANG, Tao; ZHU, Zhendong; WO2014/149164; (2014); A1;,
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