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4-chloro-3,5-difluoro-2-nitrobenzoic acid[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
94.9%
A solutionof 4-chloro-3,5-trifluorobenzonitrile (2) (5.0 g, 28.9 mmol) inconcentrated H2SO4 (98%, 92.0 g) was stirred for 1 h in an ice-bath.After being treated dropwise with the mixture of concentrated HNO3(65%, 2.0 g) and H2SO4 (98%, 2.2 g), the ice-bath was removed andthe mixture was stirred for another 6 h at about 102 . The reactionprogress was monitored by TLC (30% ethyl acetate in hexane). Aftercomplete conversion of compound 2, the reaction mixture was cooledto 0 by ice-bath, then treated dropwise with sodium nitrite solution(4.0 g in 25 mL water). After the addition, the mixture was stirred foranother 20 h at 120. The reaction progress was monitored by TLC(30% ethyl acetate in hexane). After cooling to room temperature,the reaction mixture was extracted with ethyl acetate (2×20 mL) andthe combined organic phases were dried over Na2SO4. The solventwas removed under reduced pressure to afford a white solid (6.9 g).The crude product was purified by using 20% ethylacetate:hexaneas eluent through column chromatography. The solvent was removedunder reduced pressure to afford a yellow solid 3 (6.5 g) in 94.9%yield.
Chemistry
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Material Science
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