Yield:5028-15-9 94%

Reaction Conditions:

with potassium carbonate in water;Heating / reflux;

Steps:

26

PREPARATION 26;1 -Methyl -4-(3-nitropyridin-2-yl)piperazine;.2-Chloro-3-nitropyridine (2.Og, 12.6 mmol), 1-methylpiperazine (2.1 mL, 18.9 mmol) and K₂CO₃ (3.5 g, 25.3 mmol) were refluxed overnight in water (50 mL). Following cooling, the mixture was extracted with EtOAc (2x75 mL). The extracts were washed with brine, dried (MgSO₄) and concentrated to yield 2.63 g, 94%) of PP26 as an orange oil: MS (AP/CI) 223.0 (MH⁺); NMR (CDCI₃) 8.29 (dd, J = 4.6, 1.7 Hz, 1 H), 8.08 (dd, J = 7.9, 1.7 Hz, 1 H), 6.70 (dd, J = 7.9, 4.6 Hz, 1 H), 3.45 (t, J = 5.2 Hz, 4H), 2.48 (t, J = 5.0 Hz, 4H), 2.31 (s, 3H); ¹³C NMR (CDCI₃) 152.96, 151.96, 135.82, 133.17, 113.53, 54.92, 48.13, 46.36.

References:

WO2006/48727,2006,A1 Location in patent:Page/Page column 73