These common heterocyclic compound, 67567-26-4, name is 4-Bromo-2,6-difluoroaniline, 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. Computed Properties of C6H4BrF2N
4-bromo-2,6-difluoroaniline (31.05 g, 0.15 mol)N-isopropylacetamide (30.3 g, 0.30 mmol),Phosphorus oxychloride (20.9 mL, 0.225 mol) was added successively to anhydrous toluene.Triethylamine (31.3 mL, 0.225 mol) was slowly added dropwise to the reaction flask in a constant pressure funnel under ice-Keep the internal temperature less than 60 C.The reaction flask was transferred to an oil bath and heated to solvent reflux.After 2 hours the reaction flask was cooled to room temperature,Slowly poured into a 300 g ice-water mixture,Add 300 ml of ethyl acetate,After mixing well,The aqueous layer was again extracted with 200 ml of ethyl acetate,Combined organic layer,After washing with saturated brine, dried over anhydrous sodium sulfate,Concentrated under reduced pressure to obtain a pale yellow solid,Add 100 ml of petroleum ether beating for 10 minutes,The compound of formula IX-1 (28.0 g) was filtered off under reduced pressure,As an off-white solid (yield 92.3%).
The synthetic route of 4-Bromo-2,6-difluoroaniline has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Chia Tai Tianqing Pharmaceutical Group Co., Ltd.; Zhang, Yinsheng; Liu, Yingshuai; Li, Li; Miao, Lei; Xu, Tongjie; Liu, Haiyan; Ma, Xueqin; Yu, Sen; Xu, Hongjiang; (49 pag.)CN106467517; (2017); A;,
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