3-Bromobiphenyl synthesis
- Product Name:3-Bromobiphenyl
- CAS Number:2113-57-7
- Molecular formula:C12H9Br
- Molecular Weight:233.1
Yield:2113-57-7 80.61%
Reaction Conditions:
Stage #1:iodobenzene;1-Bromo-3-iodobenzene with magnesium in tetrahydrofuran for 1 h;Inert atmosphere;Reflux;Green chemistry;
Stage #2: in tetrahydrofuran at 50 - 85; for 8 h;Green chemistry;
Steps:
3 Embodiment 3, a modified palladium can be recycled to the direct coupling of the aromatic Grignard reagent method for the synthesis of halogenated aromatic hydrocarbon, its synthesis route is as follows:
General procedure: Wherein the catalyst organic phosphine ligand complex preparation Pd/C (II) is: under the protection of inert gas, with a mechanical stirring, to the reflux condensation drying tube 100 ml three port in the reaction bottle, adding Pd/C0.3g (aqueous 56%), toluene 50 ml, the temperature is increased to 110 °C, return water 120 min, cooling to 90 °C, by adding organic ligand phosphine 4,5-didiphenyl-phosphine -9,9-dimethyl-oxa anthracene or two n-butyl (1-adamantyl) diphenylphosphinobiphenyl 0.0006mol, heating to 110 °C, stirring 60 min, cooling to 30 °C, to obtain catalyst organic phosphine ligand complex for Pd/C (II) system.(VI) is prepared by coupling aromatic hydrocarbon: under the protection of inert gas, with a mechanical stirring, refluxing condensed drying tube, of the feeding funnel 100 ml in the reaction bottle, by adding magnesium powder 0.0501mol, THF10ml, a grain joins the iodine, aromatic hydrocarbon (III) 0.0483mol instillment halogenating, usage of THF26ml, completion of the dropping, reflux reaction 2h, Grignard reagent (IV) for use.Under the protection of the inert gas, to the other is provided with a mechanical stirring, refluxing condensed drying tube, of the feeding funnel 250 ml reaction vial halogenated aromatic hydrocarbon (V) 0.0432mol to, II system by adding inactive catalyst, (IV) the above-mentioned standby Grignard reagent into the reaction system is dropping, and 50-85 °C reaction 12h, stopping reaction, filter catalyst organic ligand phosphine complex Pd/C (II), the catalyst can be recovered under, the organic phase washed to neutral, drying, column, concentration, distillation product coupling aromatic hydrocarbon (VI), main content GC analysis > 98%, the yield is > 80%. GC-MS and elemental analysis confirmed.
References:
Shandong Shenghua Electronic New Material Co., Ltd.;Wu, Shengxi;Du, Kaichang;Wu, Hua;Hou, Juan;Liang, Bin;Sun, Yonghe;Wang, Zuopeng CN105348037, 2016, A Location in patent:Paragraph 0019; 0020; 0021
108-36-1
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2113-57-7
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