Related Products of 658-99-1, These common heterocyclic compound, 658-99-1, name is 2-(3,4-Difluorophenyl)acetonitrile, 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.
Example S23; Preparation of 2-(3,4-difluoro-phenyl)-ethylamine hydrochloride; To 3.71 g of LiAlH4 (98 mmol) in 30 ml of dry diethylether were added dropwise at 0 C. under nitrogen 5 g of 3,4-difluoroacetonitrile (33 mmol) in 30 ml THF. After the addition and additional 15 min of stirring at 0 C., the ice bath was removed and the reaction was allowed to warm to ambient temperature. The flask was then immersed in an oil bath, heated to 55 C. and the reaction was refluxed overnight. The oil bath was then removed and the reaction mixture cooled to 0 C. The LiAlH4 was then quenched by the slow and sequential addition of saturated aqueous sodium sulfate solution. After the initial exothermic reaction had subsided, the flask was allowed to warm to ambient temperature and further sodium sulfate solution was added until the color was light grey. Then more solid sodium sulfate (dry) was added to dry the mixture, which was subsequently filtered through a short bed of sodium sulfate in a sinter funnel. To the filtrate was added a 5 N HCl solution in dioxane. The HCl-salt precipitated out and was filtered. The collected yellow solid (4.2 g; 82% yield) was found to be of good purity by NMR and was taken into the next step without further purification. MS (ISP) 158.1 (M+H)+.
The synthetic route of 658-99-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Conte-Mayweg, Aurelia; Kuehne, Holger; Luebbers, Thomas; Maugeais, Cyrille; Mueller, Werner; Pflieger, Philippe; US2006/30613; (2006); A1;,
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