A new synthetic route of 626-39-1

Electric Literature of 626-39-1, These common heterocyclic compound, 626-39-1, name is 1,3,5-Tribromobenzene, 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.

[0372] 1,3,5-Tribromo-benzene (31.4 g, 100 mmol) was dissolved under argon in a flame dried three-neck flask in 1000 mL diethylether and the solution was cooled to -72C. A solution of 62 mL r°BuLi (1.6 M in hexane, 100 mmol) was added to the resulting suspension in such a fashion that temperature did not rise above -7O0C. The mixture was stirred for 30 min at -750C and the reaction was monitored by HPLC. A solution of 10.4 g (100 mmol) 3-cyanopyridine in 100 mL diethylether was added in such a fashion that temperature did not rise above -710C. The mixture was stirred at -75C for 60 min and the reaction was monitored by HPLC. The cooling bath was removed and warmed to -250C. 2 N HCl (250 mL) was added and the mixture was stirred for 20 min at room temperature. The mixture was made alkaline by addition of 1 N NaOH. The product was extracted with ethyl acetate and the combined organic layers were dried over Na2SO4. The product was purified by chromatography (700 g silica agel, CH2Cl2, then CH2Cl2 / ethyl acetate 1:1, UV) to yield 27.7 g (81 %) of (3,5-dibromo-rhohenyl)-pyridin-3-yl-methanone.

The synthetic route of 626-39-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LOCUS PHARMACEUTICALS, INC.; WO2008/8059; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary