In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 327-51-5, name is 1,4-Dibromo-2,5-difluorobenzene belongs to bromides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Product Details of 327-51-5
under a nitrogen atmosphere, to a 500ml reaction vessel 2,3-dibromo-thiophene (Wako Pure Chemical Industries, Ltd.) added to 15g and THF160ml did. This solution under ice-cooling ethyl magnesium chloride (Sigma-Aldrich, 2.0M) was added to THF solution 32ml (63mmol) of, and stirred for 10 minutes at the same temperature, 3-bromothiophene-2-magnesium chloride (3-halo thiophene-2-magnesium halide) was prepared. It added another 1l reaction vessel to zinc chloride (Wako Pure Chemical Industries, Ltd.) 10g (73mmol) and THF100ml, was a fine white slurry was stirred under ice-cooling. Then 3-bromo-2-magnesium chloride in an ice-cold solution of the (water bath temperature 10 C) was transferred to the zinc chloride solution, and the mixture was stirred for 30 minutes. Further the temperature was raised to room temperature, stirred for 10 minutes, 3-bromo-2-zinc chloride (3-halo-2-zinc derivative) was prepared. To this mixture 1,4-dibromo-2,5-difluorobenzene (Wako Pure Chemical) 5.5 g (20 mmol), catalyst as tetrakis (triphenylphosphine) palladium (Tokyo Kasei Kogyo) 350 mg (0.30 mmol) (1 , it was added 1.5 mol%) on the 4-dibromo-2,5-difluorobenzene. After carrying out 25 hours cross-coupling reaction at 50 C, the reaction by the addition of water-cooled vessel 1N hydrochloric acid 90ml stopped. It was extracted with toluene and the organic phase was washed with brine, and dried with anhydrous sodium sulfate. Concentrated in vacuo, and filtered resulting residue in a small amount of silica gel, concentrated crystal was further washed with hexane. Heptane / toluene = purified by recrystallization from 2/1, to give a pale yellow solid 5.3g of 1,4-bis (3-bromo-2-thienyl) -2,5-difluoro-benzene (61% yield).
The synthetic route of 327-51-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Tosoh Corporation; Ueda, Saori; Watanabe, Masato; (7 pag.)JP2016/74626; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary