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. 1017779-69-9, name is 3-Fluoro-4-(trifluoromethoxy)aniline, A new synthetic method of this compound is introduced below., HPLC of Formula: C7H5F4NO
[0202j meta-Fluoro-4-(trifluoromethoxy)aniline (500 mg, 2.56 mmol) and triethylamine (388 mg, 3.84 mmol) were dissolved in CH2C12 (4 mL) and was added dropwisely into a solution of triphosgene (341 mg, 1.15 mmol) dissolved in CH2C12 (5 mL) at -78 C. The reaction mixture was stirred at 0 C for lh and was then cooled to -78 C. 4-amino-1-Boc- piperidine (769 mg, 3.84 mmol) and triethylamine (388 mg, 3.84 mmol) were dissolved in CH2C12 (4 mL) and the suspension was added dropwisely to the reaction mixture at -78 C. The reaction mixture was stirred at rt for 2h. The reaction was quenched by addition of water. The organic layer was isolated and the organic layer was further washed by HC1 solution (1M) for 4 times. The organic layer was dried over anhydrous magnesium sulfate and concentrated in vacuo yielding final crude product (1.05 g, 86% pure, 2.13 mmol, 83.4% yield). The impurities 38 were purified by column chromatography using EtOAc:Hex (1:1).[0203j ?H NMR (d6-DMSO, 300 Mhz): A: 8.77 (s, 1H), 7.66 (dd, J 13.5, 2.4 Hz, 1H), 7.38 (t, J 8.1 Hz, 1H), 7.10 (d, J 9Hz, 1H), 6.33 (d, J 7.5 Hz, 1H), 3.81 (d, J= 12.9 Hz, 2H), 3.6-3.8 (m, 1H), 2.8-3.0 (m, 2H), 1.78 (dd,J= 12.3Hz, 3.3Hz, 2H), 1.40 (s, 9H), 1.2-1.4 (m, 2H); 38: 9.28 (s, 1H), 7.69 (dd, J= 14.9, 2.4 Hz, 1H), 7.46 (t, J 9Hz, 1H), 7.2-7.3 (m, 1H)
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; EICOSIS, LLC; HAMMOCK, Bruce, D.; LEE, Kin, Sing, Stephen; INCEOGLU, Ahmet, Bora; WO2015/148954; (2015); A1;,
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