Electric Literature of 19752-55-7,Some common heterocyclic compound, 19752-55-7, name is 1-Bromo-3,5-dichlorobenzene, molecular formula is C6H3BrCl2, 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.
To 5.1 g (0.209 mol) of magnesium turnings were added 0.45 g of a 1 molar solution of DIBAL in hexane at 60°C. After 15 min, 3,5-dichloro-bromobenzene (5.0 g, 0.022 mol) and 25 mL THF were added and the mixture was stirred. After start up of the reaction a mixture of 45g (0.2 mol) 3,5-dichloro-bromobenzene and 250 mL THF was added under reflux. After completion of the reaction the mixture was cooled to 0°C and 31 .1 g (0.219 mol) of ethyl trifluoroacetate were added. After 2 h an aqueous solution of NH4CI was added and the mixture was separated between MTBE and aqueous N H4CI solution. The organic layer was separated and the solvent was removed in vacuum. (34.3g brown oil; purity 70percent acc. to g.c; yield 50percent)1H-NMR (360 MHz, CDCI3): delta = 7.7 (s, 1 H), 7.9 (s, 2H) ppm.
The synthetic route of 19752-55-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BASF SE; KOeRBER, Karsten; KORDES, Markus; RACK, Michael; VON DEYN, Wolfgang; KAISER, Florian; WO2012/59441; (2012); A2;,
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