Hydrochloric Acid → HCID 15550707, compound

Participants

Reaction Steps

To a solution of 1-(3-amino-6-chloro-3-nitro-pyridin-2-yl)-propan-2-ol (0.3 g, 1.67 mmol) in anhydrous THF (20 mL) was added a solution of 1,1′-carbonyldiimidazole (0.68 g, 4.12 mmol) in anhydrous THF (10 mL). The reaction mixture was heated under reflux for 3 h. The reaction mixture was treated with 0.5N HCl, washed with brine, H2O, dried (MgSO4), concentrated and crystallized from EtOAc/hexane to obtain the title compound as a white crystalline solid (0.2 g, 56%): mp 175-178° C. 1H NMR( DMSO-d6) δ1.60 (s, 6H), 7.30 (d, 1H, J=8.41 Hz), 7.41 (d, 1H, J=8.41 Hz), 10.47 (s, 1H); MS((+)APCI) m/z 213 (M+H)+; Anal. Calc. For C9H9ClN2O2: C, 50.84; H, 4.27; N, 13.17. Found: C, 50.99; H, 4.28; N, 12.98.

Provenance & Evidence