反应详情

After 1.035 g of 2-(4-chloro-2-fluoro-5-isopropoxyphenyl)-4-cyano-5-trifluoromethylpyridazin-3-one (The present compound 1-5) was dissolved in 6.0 mL of tetrahydrofuran, 3.1 mL of a diethyl ether solution of methylmagnesium iodide (0.98M diethyl ether solution) was added to the tetrahydrofuran solution at 0° C. and stirred for 20 min under a nitrogen stream. Afterwards, the reaction solution was poured into 3N-hydrochloric acid and extracted with ethyl acetate. After the organic solvent was washed with aqueous saturated sodium bicarbonate and concentrated, the residue was subjected to silica gel column chromatography (eluent: ethyl acetate/hexane=1/9) to afford 0.467 g of 2-(4-chloro-2-fluoro-5-isopropoxyphenyl)-4-methyl-5-trifluoromethylpyridazin-3-one (compound 2-5).

1. extractionextracted with ethyl acetate
2. washAfter the organic solvent was washed with aqueous saturated sodium bicarbonate
3. concentrationconcentrated