反应详情

While stirring 1.2 g of methyl 5-(4,6-dimethoxypyrimidin-2-yl)oxy-2-ethoxy-2,3-dihydrobenzofuran-4-carboxylate in 20 ml of dimethylsulfoxide at room temperature, 2 ml of a 2N sodium hydroxide aqueous solution was dropwise added thereto over a period of 10 minutes and then the mixture was further stirred for 15 hours. The mixture was poured into water and extracted with diethyl ether. Then, the aqueous layer was acidified with 10% hydrochloric acid, and precipitated crystals were extracted with ethyl acetate, and the organic layer was washed with water and then dried over anhydrous sodium sulfate. It was concentrated under reduced pressure, and the oily substance thereby obtained was purified by silica gel column chromatography (n-hexane/ethyl acetate=1/1) to obtain 1.0 g (yield: 87%) of the desired compound.

1. extractionextracted with diethyl ether
2. customprecipitated crystals
3. extractionwere extracted with ethyl acetate
4. washthe organic layer was washed with water
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationIt was concentrated under reduced pressure
7. customthe oily substance thereby obtained
8. customwas purified by silica gel column chromatography (n-hexane/ethyl acetate=1/1)