反应详情

A 40% methylamine-methanol solution (167.4 g, 2.156 mol) was added to a mixed solution of the crude ethyl α-oxo-2-(2-tetrahydropyranyloxymethyl)phenylacetate thus obtained and methanol (100 ml), and the mixture was stirred at room temperature for 40 minutes. After completion of the reaction, the mixture was concentrated under reduced pressure. Benzene (300 ml) was added to the resulting residue to filter off the insoluble materials, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to obtain N-methyl-2-oxo-2-[2-(2-tetrahydropyranyloxymethyl)phenyl]acetamide (114.8 g, Yield: 76.8%) as an oil.

1. customthus obtained
2. customAfter completion of the reaction
3. concentrationthe mixture was concentrated under reduced pressure
4. additionBenzene (300 ml) was added to the resulting residue
5. filtrationto filter off the insoluble materials
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane)