9-(2-Bromphenyl)-phenanthren synthesis
- Product Name:9-(2-Bromphenyl)-phenanthren
- CAS Number:3582-48-7
- Molecular formula:C20H13Br
- Molecular Weight:333.22
Yield:3582-48-7 72%
Reaction Conditions:
with tetrakis(triphenylphosphine) palladium(0);sodium carbonate in tetrahydrofuran;water;toluene at 90;Inert atmosphere;
Steps:
3.1; 4.1 Step 1: Synthesis of Intermediate 4
Dissolve o-dibromobenzene (23.6g, 100.0mmol) and 9-phenanthrene boronic acid (22.2g, 100.0mmol) in 200ml of toluene, then add 2M sodium carbonate aqueous solution (50.0ml), And tetrahydrofuran (50.0ml); after blowing with nitrogen to remove the air, quickly add the catalyst tetrakis(triphenylphosphine)palladium (347mg, 3.0mmol); under the protection of nitrogen, heat to 90, React overnight, then add ethyl acetate and water, stir, stand, Separate the layers, extract the organic phase, and dry over anhydrous magnesium sulfate, remove the solvent under reduced pressure, Use silica gel column chromatography, eluent is petroleum ether, and finally The pure intermediate 4 (24.0g, 72.3mmol) was obtained, The reaction yield in this step was 72%.
References:
CN108342191,2020,B Location in patent:Paragraph 0081-0085; 0098-0099
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