Application of 656-64-4,Some common heterocyclic compound, 656-64-4, name is 3-Bromo-4-fluoroaniline, molecular formula is C6H5BrFN, 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.
3-bromo-4-fluoroaniline (60 g, 315.6 mmol), acetonitrile (600 mL), water (600 mL), and concentrated hydrochloric acid (300 mL).The mixture was cooled to 0-5 C in an ice bath, and a solution of sodium nitrite (23.4 g, 316 mmol) in water (300 mL) was added dropwise, maintaining the system temperature at 0-5 C.After 1 hour of reaction, urea (3.6 g, 60 mmol) was added to quench excess sodium nitrite and stirred for 10 minutes.Sodium sulfide nonahydrate (100.8 g, 420 mmol), sulfur powder (13.2 g, 420 mmol), NaOH (17.4 g, 432 mmol), water (300 mL) were sequentially added to a 1 L three-necked flask. The oil bath was heated to 75 C for 1 hour until the solution became clear. The clear solution was cooled to room temperature and added dropwise to the above reaction liquid, and the temperature of the system was maintained at 0 to 5 C. After the completion of the dropwise addition, the reaction mixture was extracted with ethyl acetate (1L 2), filtered, dried over anhydrous sodium sulfate and evaporated to dryness to give the crude product of 1,2-bis(3-bromo-4-fluorophenyl)disulfane (42 g) , yellow oil, yield 64%).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Bromo-4-fluoroaniline, its application will become more common.
Reference:
Patent; Shanghai Hansen Bio-pharmaceutical Technology Co., Ltd.; Jiangsu Haosen Pharmaceutical Group Co., Ltd.; Ye Guozhong; Liu Lei; Bao Rudi; Wu Shenghua; Deng Haining; (130 pag.)CN110041253; (2019); A;,
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