Hydrazine hydrate (1:1) → HCID 59320406, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 4-(6-chloro-pyridazin-3-yl)-2-fluoro-N-methyl-benzamide 34 g (128 mmol) in 500 mL of dry pyridine was cooled in an ice bath and 43.5 mL of hydrazine hydrate was added. The cooling was continued so as to keep the temperature below 30° C. at which time yellow needle separated. The mixture was then heated to 65° C. and stirred overnight. The mixture was filtered and the solid washed with water and Methanol to return the title compound (28.8 g, 84% yield) as a light yellow solid. 1H NMR (300 MHz, DMSO-d6): δ (ppm): 8.27 (s, 2H), 7.96˜7.99 (d, 1H), 7.86˜7.92 (m, 2H), 7.69˜7.75 (m, 1H), 7.09˜7.12 (d, 1H), 4.42 (s, 2H), 2.78˜2.80 (d, 3H); MS (m/z): 262.1 [M++1].

Provenance & Evidence