Synthetic Route of 31604-30-5,Some common heterocyclic compound, 31604-30-5, name is 1,2,4,5-Tetrabromo-3,6-dichlorobenzene, molecular formula is C6H7N5O, 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.
In an argon flushed Schlenk flask a mixture of magnesium turnings (3.6 g, 150 mmol), 1,2 dibromoethane (0.2 mL) and 10 mL of dry THF was stirred at 45-50 C for a few minutes. After the reaction ceasing, the solution was removed via cannulation and dry THF (100 mL) was added. Then, a solution of 1-bromo-4-(3,7-dimethyloctyl)benzene (22 g, 100 mmol) was slowly added at room temperature and the reaction mixture was stirred for 24 h at 80 C. The gray solution of 4-(3,7-dimethyloctyl)phenyl magnesium bromide was then transformed into a suspension of 1,4-dichloro-2,3,5,6-tetrabromobenzene (4.6 g, 10 mmol) in 20 mL of dry THF under argon and the resulting mixture was stirred at 80 C for 24 h. I2 (25 g, 100 mmol) was mixed directly to the reaction mixture at 0 C and the reaction was stirred at 80 C under argon for 4 h. The reaction was quenched with water and the resulting mixture was extracted with CHCl3 (100 mL ¡Á 3). The combined organic layers were washed with 2 M aqueous NaHSO3 solution (200 mL ¡Á 2) and brine (50 mL), dried with MgSO4 and concentrated in vacuum. The residue was purified with chromatography (Silica gel, CH3(CH2)4CH3/CH2Cl2 = 20/1) to give 7.7 g of compound I as a thick oil. The yield is 65%.
The synthetic route of 31604-30-5 has been constantly updated, and we look forward to future research findings.
Reference:
Article; Patil, Siddappa A.; Uthaisar, Chananate; Barone, Veronica; Fahlman, Bradley D.; Journal of Molecular Structure; vol. 1032; (2013); p. 41 – 47;,
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