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912444-99-6

2-amino-5-fluoro-3-nitrobenzonitrile synthesis

2synthesis methods
-

Yield:912444-99-6 89%

Reaction Conditions:

tetrakis(triphenylphosphine) palladium(0) in N,N-dimethyl-formamide at 95; for 22 h;

Steps:

51B

EXAMPLE 51B; 2-Amino-5-fluoro-3-nitro-benzonitrile A suspension of Example 51A (35.0 g, 0.15 mol), zinc cyanide (34.98 g, 0.3 mol) and tetrakis(triphenylphosphine)palladium (0) (12.05 g, 10 mmol) in anhydrous DMF (420 mL) was heated under nitrogen at 95° C. for 22 h. After cooling, insoluble material was filtered off and the filtrate was partitioned between ethyl acetate and brine. The organic phase was washed with water and concentrated. The residual solid was recrystallized from methanol to provide Example 51B (24 g, 89%). MS (DCI/NH3) m/z 182 (M+H)+.

References:

US2006/229289,2006,A1 Location in patent:Page/Page column 25