反应详情

温度

100 °C

A suspension of starting material 6-chloro-3-hydrazinylpyridazine-4-carboxylic acid (4.80 g, 26 mmol) in acetic acid (100 mL) was heated at 100° C. for 3 hours. The mixture was cooled to room temperature, concentrated in vacuum to give the crude product, which was washed by PE (50 mL) first, then recrystallized from MeOH to give product 6-chloro-3-methyl-[1,2,4]triazolo[4,3-b]pyridazine-8-carboxylic acid as a yellow solid (4.00 g, 72.5%). 1H NMR (300 MHz, DMSO) δ: 7.2 (s, 1H), 2.66 (s, 3H). LRMS (M+H+) m/z: calcd 213; found 213.

1. temperatureThe mixture was cooled to room temperature
2. concentrationconcentrated in vacuum
3. customto give the crude product, which
4. washwas washed by PE (50 mL) first
5. customrecrystallized from MeOH