Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 851386-40-8, name is 4-Chloro-2,5-difluoropyridine. This compound has unique chemical properties. The synthetic route is as follows. Safety of 4-Chloro-2,5-difluoropyridine
Diisopropylamine (30 g, 0.29 mol) was dissolved in anhydrous tetrahydrofuran (200 ml) and the nitrogen was removed.Cooling to -65 – 40 ,A solution of n-butyllithium / n-hexane (2.5 M, 105 ml)Stir the mixture for 30 minutes.4-chloro-2,5-difluoropyridine (50 g, 0.33 mol) obtained in the above step was slowly added dropwise at -65 C,After the dropwise addition, the mixture was stirred for 1 hour.A solution of methyl iodide (42 g, 0.29 mol)Dripping finished slowly rose to -50 ,And stirred for 1 hour,TLC reaction is complete.The reaction was quenched with saturated ammonium chloride solution,Methyl tert-butyl ether extraction reaction solution,The organic phase was washed with 2N hydrochloric acid,Then washed with water,Saturated sodium bicarbonate wash,Saturated with salt water,The organic phase was separated and dried over anhydrous sodium sulfate,filter,The filtrate was distilled off at 80 C to 120 C under atmospheric pressure,The remaining crude product at 0.09MPa at 70 ~ ~ 100 vacuum distillation of the product,A fraction of 65-80 C was collected to give the product 4-chloro-2,5-difluoro-3-methylpyridine (34.8 g, yield 64%).
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Reference:
Patent; Danuo Pharmaceutical (Suzhou) Co., Ltd.; Ding, Jun; He, Shijie; Zhuang, Zhijun; Ma, Zhenkun; (13 pag.)CN106432222; (2017); A;,
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