1-(2-FLUORO-4-NITROPHENYL)-1H-1,2,4-TRIAZOLE synthesis

Yield:182060-01-1 90%

Reaction Conditions:

with potassium hydrogencarbonate in DMF (N,N-dimethyl-formamide) at 80; for 1 h;

Steps:

34

To a suspension of anhydrous potassium bicarbonate (8.30 grams, 60 mmol) in DMF (50 mL) was added 3, 4-difluoronitrobenzene (5.0 grams, 31.4 mmol) followed by the addition of [1, 2, 4]-triazole (2.6 grams, 37.6 mmol) and heated to 80 °C for 1 hours. The reaction mixture was poured onto crushed ice and the precipitate was filtered off. It was then washed with water and dried under vacuum to yield the title compound as white solid (5.85 grams, 90%). 1H NMR (CDC13) : No. 8.85 (s, J= 2.4 Hz, 1H), 8.32-8. 11 (M, 4H); MS (mle) : 209 (M++1), 195; IR (KBR, CM-1) : 1533, 1510 ; 1346.

References:

WO2004/101531,2004,A1 Location in patent:Page 65