反应详情

To a mixed solution of ethyl [[[[5-[(2,5-difluorophenyl)[(4-fluorophenyl)sulfonyl]methyl]-4-methylpyridin-2-yl]carbonyl]amino]methoxy]acetate (167 mg, 0.311 mmol) in tetrahydrofuran (6 ml) and water (3 ml), lithium hydroxide monohydrate (16 mg, 0.373 mmol) was added, and the mixture was stirred for 20 hours at room temperature. 1 N hydrochloric acid (0.5 ml) and water were added to the reaction solution, and the mixture was extracted with methylene chloride. The organic layer was dried over anhydrous sodium sulfate and filtered, and then the filtrate was concentrated under reduced pressure. The resulting concentration residue was subjected to flash silica gel column chromatography, and the fraction obtained from an elution with methanol:methylene chloride (=1:10) was concentrated under reduced pressure. A mixed solution of ethyl acetate-hexane was added to the resulting concentration residue, and then the residue was collected by filtration to obtain the title compound (38 mg, 0.075 mmol, 24%) as a white powder.

1. extractionthe mixture was extracted with methylene chloride
2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
3. filtrationfiltered
4. concentrationthe filtrate was concentrated under reduced pressure
5. concentrationThe resulting concentration residue
6. customthe fraction obtained from an elution with methanol
7. concentrationmethylene chloride (=1:10) was concentrated under reduced pressure
8. additionA mixed solution of ethyl acetate-hexane was added to the resulting concentration residue
9. filtrationthe residue was collected by filtration