In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 1-Bromo-3,4,5-trifluorobenzene
5-Bromo-1,2,3-trifluorobenzene (19.855 g, 94.110 mmol) was added slowly dropwise to a chilled (-85 to -80 C. (liquid nitrogen/acetone)) solution of n-butyllithium (9.10 mL, 2.38 M, 21.7 mmol combined with 45.5 mL, 1.57 M, 71.4 mmol; total: 93.1 mmol) in ether (200 mL) such that the temperature did not exceed -89 C. The temperature was allowed to increase to between -78 and -75 C. for 2.5 hours (dry ice bath) with formation of white precipitate. The reaction mixture was cooled to -85 C. A solution of dimethylphosphoramidous dichloride (6.791 g, 46.53 mmol) in ether (10 mL) was added very slowly dropwise such that the temperature did not exceed -80 C. Dry ice was added to the bath and the reaction mixture was allowed to stir overnight while warming to ambient temperature. 31P and 19F NMR spectra showed the product to be about 99.5% desired product. The reaction mixture was filtered and the volatiles were removed under reduced pressure. The residue was extracted with hexane, filtered, and the volatiles were removed under reduced pressure to give 5 as a pale yellow oil, 13.50 g, 86.04%. 1H NMR (500 MHz, CDCl3) delta 6.95 (dt, J=7.5, 6.4 Hz, 4H), 2.64 (d, J=9.7 Hz, 6H). BC NMR (101 MHz, CDCl3) delta 151.35 (dddd, J=254.1, 10.0, 8.2, 3.0 Hz), 140.00 (dtd, J=254.5, 15.5, 2.2 Hz), 134.44 (dq, J=21.9, 3.7 Hz), 115.41 (ddd, J=21.7, 15.1, 5.5 Hz), 41.47 (d, J=16.3 Hz). 31P NMR (202 MHz, CDCl3) delta 65.05. 19F NMR (376 MHz, CDCl3) delta -133.39–133.55 (m), -159.17 (ttd, J=20.3, 6.7, 3.4 Hz).
The synthetic route of 138526-69-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Dow Global Technologies LLC; Klosin, Jerzy; Milbrandt, Kara A.; Boelter, Scott D.; Wilson, David R.; Rosen, Mari S.; Welsh, Dean M.; Margl, Peter M.; Koh, Kyoung Moo; Pearson, David M.; Huacuja, Rafael; (191 pag.)US2018/291048; (2018); A1;,
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