3-AMINO-1-(4-NITROPHENYL)-1H-PYRAZOLE-4-CARBONITRILE synthesis

Yield:219930-67-3 77%

Reaction Conditions:

with potassium carbonate in dimethyl sulfoxide at 20; for 64 h;

Steps:

35.a (a)

(a) 3-amino-4-cyano-1-(4-nitro-phenyl)-1H-pyrazole 5.50 g (50.9 mmol) 3-amino-4-cyano-1H-pyrazole are stirred together with 7.54 g (53.4 mmol) 4-fluoro-1-nitro-benzene and 8.44 g (61.1 mmol) potassium carbonate in 50 ml DMSO for 64 h at ambient temperature. Then the mixture is poured into 1800 ml of water and stirred for 20 min. Then it is suction filtered, the filter cake is dried, stirred in ethyl acetate, filtered off and dried again. Yield: 9.00 g (39.3 mmol, 77%) C₁₀H₇N₅O₂ (229.20) Mass spectrum: (M-H)^-=228

References:

US2008/51578,2008,A1 Location in patent:Page/Page column 50