Synthetic Route of 399-94-0, These common heterocyclic compound, 399-94-0, name is 1-Bromo-2,5-difluorobenzene, 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.
Under nitrogen, 2,5-difluorobromobenzene (15.05 g, 78 mmol) was dissolved in dry toluene (50 mL)(66 mL, 1.3 mol / L), and the mixture was stirred at about -10 C for 1 hour, and the mixture was cooled to -10 C or lower and the isopropylmagnesium chloride / lithium chloride tetrahydrofuran solution (66 mL, 1.3 mol / L) was added dropwise.1D (10 g, 39 mmol) was dissolved in dry tetrahydrofuran (100 mL) and added dropwise to the above reaction solution. The temperature was maintained below -10 C and the reaction was carried out at room temperature for 4 hours. The temperature was reduced to below -10 C, saturated ammonium chloride solution (40 mL) was added dropwise, stirred for 10 minutes, adjusted to pH 5 to 6 with 3 mol / L hydrochloric acid solution, The organic phase was washed with saturated sodium chloride solution (30 mL x 2). The organic phase was dried over anhydrous sodium sulfate, filtered and concentrated, and the column was separated by column chromatography. (Petroleum ether / ethyl acetate (nu / nu) = 50: 1 -8: 1) to give 1E as a pale yellow solid (10.1 g, yield 83.5%).
Statistics shows that 1-Bromo-2,5-difluorobenzene is playing an increasingly important role. we look forward to future research findings about 399-94-0.
Reference:
Patent; SICHUAN HAISCO PHARMACEUTICAL CO., LTD; FAN, JIANG; FENG, JIAN-CHUAN; PENG, FEI; CHEN, QING-PING; (89 pag.)TW2017/8224; (2017); A;,
Bromide – Wikipedia,
bromide – Wiktionary