4-NITROPYRIDINE-2-CARBOXAMIDE synthesis

Yield:62020-02-4 100%

Reaction Conditions:

with chloro-trimethyl-silane;water at 20; for 1 h;

Steps:

99A

4-Nitropicolinonitrile (100 mg, 0.67 mmol), chlorotrimethylsilane (0.17 mL, 1.4 mmol) and H₂O (0.024 mL, 1.4 mmol) was sonicated in a sonicator at rt for 1.0 h. It was diluted with EtOAc, washed with NaHCO₃, brine and dried over Na₂SO₄. After removal of solvent, 99A (134 mg, 100% yield) was obtained as a solid. ¹H NMR (400 MHz, Methanol-d₄) δ ppm 8.29 (dd, J=5.27, 2.20 Hz, 1H) 8.74 (d, J=2.20 Hz, 1H) 8.98 (d, J=5.27 Hz, 1H).

References:

US2010/227894,2010,A1 Location in patent:Page/Page column 76