Reference of 1017779-69-9, A common heterocyclic compound, 1017779-69-9, name is 3-Fluoro-4-(trifluoromethoxy)aniline, molecular formula is C7H5F4NO, 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.
A solution of 3-fluoro-4-(trifluoromethoxy)aniline [CAS 101 7779-69-9] (32.0 g, 164 mmol) in CH3CN (600 mL) was stirred on an ice-bath. N-iodo-succinimide (40.59 g, 180.4 mmol) was added and the reaction mixture was allowed to slowly reachroom temperature while stirring overnight. The solvent was concentrated under reduced pressure. Water was added and the product was extracted with EtOAc (2x 300 mL). The combined organic layers were washed with and an aqueous solution of Na2S2O3 (500 mL), brine (500 mL), dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by columnchromatography on silica gel (eluent: petroleum ether/EtOAc gradient 50/1 to30/1). The desired fractions were combined and evaporated under reduced pressure to provide 5-fluoro-2-iodo-4-(trifluoromethoxy)aniline 7a (45 g).
The synthetic route of 1017779-69-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; JANSSEN PHARMACEUTICALS, INC.; KATHOLIEKE UNIVERSITEIT LEUVEN; BARDIOT, Dorothee Alice Marie-Eve; BONFANTI, Jean-Francois; KESTELEYN, Bart Rudolf Romanie; MARCHAND, Arnaud Didier M; RABOISSON, Pierre Jean-Marie Bernard; (91 pag.)WO2017/167950; (2017); A1;,
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