Some common heterocyclic compound, 144797-57-9, name is 4-Chloro-3,5-difluorobenzonitrile, molecular formula is C7H2ClF2N, 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. Recommanded Product: 144797-57-9
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.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 144797-57-9, its application will become more common.