Electric Literature of 69902-83-6, A common heterocyclic compound, 69902-83-6, name is 1-Bromo-2-methyl-3-(trifluoromethyl)benzene, molecular formula is C8H6BrF3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Step 1[00293] To a solution of l-bromo-2-methyl-3-(trifluoromethyl)benzene (CXXVII) (5.7 g, 23.86 mmol) in CC14 (50 niL) was added NBS (4.24 g, 23.86 mmol) and a catalytic amount of benzoyl peroxide. The reaction mixture was gently refluxed for 1 h. The reaction mixture was cooled to room temperature and the precipitate was removed by filtration. The solution was concentrated under reduced pressure and the crude product was dissolved in hexane and additional precipitate was removed by filtration. The filtrate was concentrated to dryness to give l-bromo-2-(bromomethyl)-3-(trifluoromethyl)benzene (CXXVIII) as an orange oil (7.51 g, 23.62 mmol). 1H NMR (DMSO-d6) delta ppm 4.73 (s, 2H), 7.4 (dd, J=8 Hz, J=8 Hz, 1H), 7.80 (d, J=8 Hz, 1H), 8.02 (d, J=8 Hz, 1H); 19 F NMR (DMSO-d6) delta ppm -57.85 (s, 3F). The crude product was used without further purification for step 2.
The synthetic route of 69902-83-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; REMPEX PHARMACEUTICALS, INC.; GLINKA, Tomasz; HIGUCHI, Robert; HECKER, Scott; EASTMAN, Brian; RODNY, Olga; WO2012/109164; (2012); A1;,
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