Reference of 393-37-3, These common heterocyclic compound, 393-37-3, name is 5-Bromo-2-fluorobenzotrifluoride, 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.
To a solution of 4-bromo-l-fluoro-2-(trifluorom ethyl )benzene (5.0 g, 20.5 mmol, 2.9 mL) in THF (50.0 mL) was added LDA (2 M, 13.3 mL) at -78C. The mixture was stirred at -78C for 1 hr. Then DMF (1.8 g, 24.6 mmol, 1.9 mL) was added and stirred for 1 h at -78C. The mixture was poured into Sat H4C1 (20.0 mL) and extracted with ethyl acetate (20.0 mL x 3). The combined organic layers were washed with brine (20.0 mL x 3), dried over Na2S04, filtered and concentrated under reduced pressure to give a residue. The residue was purified by column chromatography (Si02, Petroleum ether / Ethyl acetate = 1/0 to 10/1) to afford 5-bromo- 2-fluoro-3-(trifluoromethyl)benzaldehyde (4 g, 14.7 mmol, 71.7% yield). 1H MR (CHLOROFORM-d, 400 MHz): delta 10.35 (s, 1H), 8.19 (dd, J= 2.5, 5.4 Hz, 1H), 7.98 (dd, J= 2.1, 6.1 Hz, 1H).
The synthetic route of 393-37-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; QUENTIS THERAPEUTICS, INC.; VACCA, Joseph P.; LI, Dansu; BETTIGOLE, Sarah; (184 pag.)WO2018/222918; (2018); A1;,
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