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ChemicalBook CAS DataBase List 3,3'-Difluorobenzophenone

3,3'-Difluorobenzophenone synthesis

11synthesis methods
-

Yield:345-70-0 87.3%

Reaction Conditions:

Stage #1: 3-fluorobromobenzenewith n-butyllithium in tetrahydrofuran at -78; for 1 h;Inert atmosphere;
Stage #2: 3-fluoro-N-methoxy-N-methylbenzamide in tetrahydrofuran at 20; for 16 h;

Steps:

16

10265] To a solution ofG-3 (133 g, 764 mmol) in THF (1 E)at -78°C. under N2 atmosphere, was added n-l3uEi (305 mE,764 mmol) dropwise over 1 h. The solution was treated with a solution of G-2 (100 g, 546 mmol) in THF. Afier addition, the mixture was slowly warmed toRT and stirred for 16 h. The solution was quenched with water (1 E) and extracted with EtOAc (3x400 mE). The combined organic layers were driedover with Na2504, filtered and concentrated. The residue waspurified by silica gel column chromatography (PE:EtOAc=50:1) to provide G-4 as a white solid (104 g, yield:87.3%).

References:

US2015/72982,2015,A1 Location in patent:Paragraph 0263; 0265

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