反应详情

温度

150 °C

Zinc chloride (820 mg, 6 mmol) was added to a stirred mixture of benzaldehyde (6.11 ml, 60 mmol) and 3-methylpyridazine (2.83 g, 30 mmol) and the resulting mixture heated for 20 hours at 150° C. The cool reaction mixture was partitioned between dichloromethane (40 ml) and 2M aqueous sodium hydroxide solution (20 ml), then the organic phase separated, combined with a dichloromethane extract (80 ml) of the aqueous phase, dried (Na2SO4) and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel, using dichloromethane: methanol (99:1) as eluant, to give the title compound (59%) as a solid. δ (CDCL3): 7.12 (1H,d), 7.34 (3H,m), 7.56 (2H,d), 7.72 (1H,d), 8.37 (1H,s), 8.50 (1H,s), 8.60 (1H,s). LRMS: m/z 183 (M+1)+.

1. customThe cool reaction mixture
2. customwas partitioned between dichloromethane (40 ml) and 2M aqueous sodium hydroxide solution (20 ml)
3. customthe organic phase separated
4. extractionextract (80 ml) of the aqueous phase
5. dry with materialdried (Na2SO4)
6. customevaporated under reduced pressure
7. customThe residue was purified by column chromatography on silica gel