ChemicalBook CAS DataBase List 2-Bromo-9,9-diphenyl-9H-fluorene

2-Bromo-9,9-diphenyl-9H-fluorene synthesis

7synthesis methods

Product Name:2-Bromo-9,9-diphenyl-9H-fluorene
CAS Number:474918-32-6
Molecular formula:C25H17Br
Molecular Weight:397.31

2-Bromo-9,9-diphenylfluorene is an aromatic hydrocarbon derivative and can be used as a pharmaceutical intermediate. It is synthesised from 2-Bromo-9-phenyl-9H-fluoren-9-ol and Benzene by substitution reaction. The reaction conditions are with aluminum (III) chloride;trifluoroacetic acid,Inert atmosphere.

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Yield:474918-32-6 98.6%

Reaction Conditions:

with aluminum (III) chloride;trifluoroacetic acid at 45 - 75; for 5.5 h;Inert atmosphere;Temperature;

Steps:

2 Synthesis of 2-bromo-9,9-diphenylfluorene

1) 10 mmol trifluoroacetic acid, 1.5 mmol anhydrous aluminum trichloride and 150 mmol dry benzene in a flaskMix well A liquid;2) 10 mmol of 2-bromo-9-phenyl-fluorene-9-ol and 90 mmol of dry benzene were mixed to give B solution;3) B was added dropwise to Solution A while stirring under argon, 2-bromo-9-phenyl-fluorene-9-ol in Solution BAnd A liquid trifluoroacetic acid molar ratio of 1: 1, mixing process control system temperature does not exceed 45 ;4) the system temperature to 75 , the reaction 1.5 h; and then maintain the system temperature and add 5 mmol trifluoroacetic acid; continueReaction 4h after the end of the reaction.5) separation and purification to be 2-bromo-9,9-diphenylfluorene, separation and purification operation: the reaction after the end of the system to join250 mmol of ice water; stratified, the organic phase was neutralized with saturated sodium bicarbonate to pH, extracted with ethyl acetate, and the extract was concentrated to give a white solid powder product with a yield of 98.6%.

References:

CN105016968,2017,B Location in patent:Paragraph 0031; 0032; 0033; 0034; 0035; 0036; 0037

591-50-4 Synthesis