反应详情

温度

95 °C

0.43 g of methyl N-[2-methyl-5-(1-hydroxyiminoethyl)benzyl]carbamate was dissolved in 15 ml of N,N-dimethylformamide, 0.75 g of potassium carbonate and 0.32 g of 2-chloro-6-methylpyridine hydrochloride were added thereto, followed by stirring under heating at from 90 to 100° C. for 8 hours. After completion of the reaction, the reaction solution was poured into water, extraction with ethyl acetate was carried out, followed by washing with water, and the organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (Wakogel C-200, eluent: hexane/ethyl acetate=4/1) to obtain 0.30 g of methyl N-{2-methyl-5-[1-(6-methylpyridin-2-yl methoxy)iminoethyl]benzyl}carbamate (m.p. 72-75° C.) as pale yellow crystals.

1. customAfter completion of the reaction
2. washby washing with water
3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
4. distillationThe solvent was distilled off under reduced pressure
5. customthe residue was purified by silica gel column chromatography (Wakogel C-200, eluent: hexane/ethyl acetate=4/1)