3-FLUORO-5-NITROBENZAMIDE synthesis

Yield:1208075-03-9 36%

Reaction Conditions:

with sulfuric acid;water;trifluoroacetic acid at 70; for 24 h;

Steps:

S.1

Step 1To a solution of 3-fluoro-5-nitrobenzonitrile (1.0 g, 6.02 mmoL) in TFA (8 mL) was added water (1 mL) and cone, sulfuric acid (2 mL). The reaction mixture was heated to 70 °C and stirred for 24 h. Then the reaction mixture was cooled to 0 °C and liquid ammonia solution was added. The solidified solid was filtered through Celite (diatomaceous earth) and washed with water to obtain 3-fluoro-5-nitrobenzamide (0.400 g, 36%>) as an off white solid. Observed mass (M-l): 183.02.

References:

WO2011/103196,2011,A1 Location in patent:Page/Page column 106