Electric Literature of 103-64-0,Some common heterocyclic compound, 103-64-0, name is (2-Bromovinyl)benzene, molecular formula is C8H7Br, 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.
Example 35; [0145] 1 ,3-Bis(2,4,6-trimethylylphenyl)-4-phenyl- 1H- 1 ,2,3-triazoliumhexafiuorophosphate (lOba), alternate preparation. To a stirred suspension of triazene 8b (5.63 g, 20 mmol) and anhydrous potassium hexafiuorophosphate (3.68 g, 10 mmol) and beta- bromostyrene 11a (mixture of isomers, 5.13 mL, 40 mmol) in dry dichloromethane (100 mL) in the dark at -78C is added tert-butyl hypochlorite (3.33 mL, 30 mmol), upon which the mixture instantly darkens. The mixture is stirred overnight as it is slowly allowed to warm to room temperature. The contents are then filtered, and the solid residue is washed with dichloromethane. The filtrate is collected, and volatiles are evaporated under reduced pressure. Diethyl ether is then added, and the mixture is vigorously triturated for ca. Ihour, with occasional scratching of the glass surfaces to ensure efficient mixing. Filtration and washing with copious quantities of diethyl ether afford, after drying under vacuum, triazolium salt lOba as an off-white solid (10.21 g, 97%). Analytical samples were obtained after recrystallization by vapor diffusion of diethyl ether in an acetonitrile solution of lOba. Characterization data are identical as for lOba prepared by the first method.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route (2-Bromovinyl)benzene, its application will become more common.
Reference:
Patent; THE REGENTS OF THE UNIVERSITY OF CALIFORNIA; BERTRAND, Guy; GUISADO-BARRIOS, Gregorio; BOUFFARD, Jean; DONNADIEU, Bruno; WO2011/139704; (2011); A2;,
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