反应详情

A solution of diethyl 2-(6-chloropyridazin-3-yl)-2-methylmalonate (19.8 g, 69.1 mmol) and LiOH (3.31 g, 138 mmol) in MeOH:Water (3:1, 200 mL) was stirred at 25° C. for 3 hrs. MeOH was removed from the reaction via rotary evaporation, and the resulting residue was reconstituted in H2O (300 mL). The aqueous mixture was washed with Et2O (3×100 mL) and then lyophilized to dryness to provide lithium 2-(6-chloropyridazin-3-yl)propanoate 48B in quantitative yield. The material was used without further work-up. 1H NMR (400 MHz, DMSO-d6) δ ppm 1.36 (3 H, d, J=7.33 Hz) 3.63 (1 H, q, J=7.24 Hz) 7.71 (2 H, s). ESI-MS:m/z 187.0 (M+H)+.

1. customMeOH was removed from the reaction via rotary evaporation
2. washThe aqueous mixture was washed with Et2O (3×100 mL)