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ChemicalBook CAS DataBase List B-[9,9-Bis(4-methylphenyl)-9H-fluoren-2-yl]boronic acid

B-[9,9-Bis(4-methylphenyl)-9H-fluoren-2-yl]boronic acid synthesis

2synthesis methods
-

Yield:1193104-83-4 65%

Reaction Conditions:

Stage #1:2-bromo-9,9-di-p-tolyl-9H-fluorene with n-butyllithium in tetrahydrofuran at -78; for 1 h;Inert atmosphere;
Stage #2:Trimethyl borate in tetrahydrofuran at 20;Inert atmosphere;
Stage #3:water with hydrogenchloride in tetrahydrofuranInert atmosphere;

Steps:

6.3 (3) Synthesis of Compound Represented by Formula 146-c
35 g (82 mmol) of [Formula 146-b] in a 500 ml round bottom flask,280 ml of tetrahydrofuran was added, cooled to -78 ° C in a nitrogen atmosphere, and 61.7 ml (99 mmol) of normal butyllithium was added to the cooled solution.Was added dropwise.After stirring for 1 hour at the same temperature, 12 g (115 mmol) of trimethylborate was added dropwise and stirred at room temperature to terminate the reaction and acidified with 2N hydrochloric acid. The reaction solution was extracted with ethyl acetate and water, the organic layer was separated, concentrated under reduced pressure, crystallized by addition of hexane, and the resulting solid was filtered to yield 21 g (yield: 65%) of the compound represented by Chemical Formula 146-c. .

References:

SFC Ltd.;Park Seok-bae;Lee Se-jin;Kim Jeong-su KR101996647, 2019, B1 Location in patent:Paragraph 0441; 0454-0459

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