反应详情

温度

65 °C

3,4-Dichloro-6-phenylpyridazine was synthesized from -oxobenzenebutanoic acid and 1-(phenylmethyl)hydrazine in 2 steps according to a procedure by Sircar (Sircar, I. J. Het. Chem. 1983, 20, 1473-1476.) 3,4-Dichloro-6-phenylpyridazine (100 mg, 0.44 mmol) was combined with sodium methoxide (1.1 mL of a 0.50M solution in methanol, 0.55 mmol, 1.25 equiv.) and methanol (296 μl, 1.5M) in a resealable tube and heated to 65° C. for 1 hour. The methanol was evaporated in vacuo, and water was added to the residue. The mixture was extracted with DCM, dried over K2CO3, filtered and concentrated in vacuo, to afford 3,4-dimethoxy-6-phenylpyridazine and 3-methoxy-4-chloro-6-phenylpyridazine, the title compound, as a solid.

1. customThe methanol was evaporated in vacuo, and water
2. additionwas added to the residue
3. extractionThe mixture was extracted with DCM
4. dry with materialdried over K2CO3
5. filtrationfiltered
6. concentrationconcentrated in vacuo