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ChemicalBook CAS DataBase List 4-Bromo-9H-fluoren-9-one

4-Bromo-9H-fluoren-9-one synthesis

10synthesis methods
-

Yield:4269-17-4 80%

Reaction Conditions:

with sulfuric acid;acetic acid for 12 h;Reflux;

Steps:

3 Example 3

To a 500 mL reaction flask, 50 mL of benzonitrile was added successively,70.7 g (0.3 mol) of o-dibromobenzene,68.4 g (0.45 mol) of cesium fluoride,Catalyst purged with argon was added bis (dibenzylideneacetone) palladium 0.86g (15mmol),Thiophene-2-carboxylate 2.86 g (15 mmol)And 7.0 g (15 mmol) of 1,1'-bis (di-t-butylphosphine) ferrocene,150 reaction 24h,filter,The filtrate was distilled to remove benzonitrile to give crude 2-bromo-2'-carbonitrile biphenyl.A 500 mL reaction flask was charged with crude 2-bromo-2'-carbonitrile biphenyl,Glacial acetic acid 80mL,Concentrated sulfuric acid 80mL.After heating and refluxing for 12 h,Cooled to room temperature,filter,To give a dark yellow solid,100 mL of water,100 mL of methanol,Recrystallization from 200 mL of cumene afforded 61.9 g of 4-bromofluorenone as a yellow solid in 80% yield.

References:

CN105237379,2016,A Location in patent:Paragraph 0006; 0016

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