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1-(3-Fluoro-5-nitrophenyl)ethanone synthesis

1synthesis methods
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Yield:7087-61-8 96%

Reaction Conditions:

with (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride in toluene at 100; for 3 h;Inert atmosphere;

Steps:

1 Step 1: l-(3-fluoro-5-nitro-phenyl)ethanone

Mix l-fluoro-3-iodo-5-nitro-benzene (lg, 3.75 mmol), tributyl(l-ethoxyvinyl)stannane (1.5 g, 4.15 mmol) and Pd(dppf)Cl2 (78 mg, 0.1 mmol) in toluene (5 mL) under N2. Stir at 100°C under N2 atmosphere for 3 hrs. Cool to room temperature, add IN HCl solution (5 mL) and stir for 20 min. Load directly onto silica gel column and purify by chromatography (EtOAc:PE=3:7) to give the title compound (660 mg, 96%).

References:

WO2014/418,2014,A1 Location in patent:Page/Page column 92