Extracurricular laboratory: Synthetic route of C6H3BrF2

The synthetic route of 399-94-0 has been constantly updated, and we look forward to future research findings.

399-94-0, name is 1-Bromo-2,5-difluorobenzene, belongs to bromides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Product Details of 399-94-0

Under nitrogen, 2,5-difluorobromobenzene (15.05 g, 78 mmol) was dissolved in dry toluene (50 mL)(66 mL, 1.3 mol / L) in an isopropylmagnesium chloride / lithium chloride solution was added dropwise to the temperature below -10 C, and the mixture was stirred at about -10 C for 1 hour. A solution of 1D (10 g, 39 mmol) in dry tetrahydrofuran (100 mL) was added dropwise to the reaction solution, maintaining the temperature at -10 C, and the reaction was carried out at room temperature for 4 hours. The temperature was reduced to about -10 C, and the saturated ammonium chloride solution (40 mL) was added dropwise. The mixture was stirred for 10 minutes. The pH was adjusted to 5 to 6 with 3 mol / L hydrochloric acid solution, (50 mL x 2). The organic phases were combined and washed with saturated sodium chloride solution (30 mL x 2). The organic phase was dried over anhydrous sodium sulfate, filtered, concentrated, and column chromatography (petroleum ether / Ethyl acetate (v / v) = 50: 1-8: 1),To give light yellow solid 1E (10.1 g, yield 83.5%).

The synthetic route of 399-94-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sichuan Haisco Pharmaceutical Co.,Ltd.; FAN, JIANG; ZHANG, CHEN; PENG, FEI; WU, YE; FENG, JIANCHUAN; WANG, JIANMIN; ZHENG, SUXIN; WEI, YONGGANG; YE, FEI; (350 pag.)TW2017/8220; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary