反应详情

To a suspension of 1-acetyl-4-[(4-isopropoxyphenyl)-methyl]-5-methyl-3-(2,3,4,6-tetra-O-pivaloyl-β-D-glucopyranosyloxy)-1H-pyrazole (1.00 g) in methanol (10 mL) was added potassium bicarbonate (0.038 g) under stirring at room temperature. The suspension turned into a solution by heating to reflux, and the mixture was stirred for further 2 hours. After confirming the completion of the reaction, a solution of glacial acetic acid (0.022 g) in water (10 mL) was added to the mixture at 60° C. to precipitate the crystals. The suspension was cooled to room temperature, and stirred under ice-cooling for 1 hour. The crystals were collected by filtration, and the obtained crystals were washed with a mixed solution of 2-propanol and n-heptane, and dried under reduced pressure to give 4-[(4-isopropoxyphenyl)methyl]-5-methyl-3-(2,3,4,6-tetra-O-pivaloyl-β-D-glucopyranosyloxy)-1H-pyrazole (0.890 g).

1. temperatureby heating
2. temperatureto reflux
3. stirringthe mixture was stirred for further 2 hours
4. customthe completion of the reaction
5. customto precipitate the crystals
6. temperatureThe suspension was cooled to room temperature
7. stirringstirred under ice-
8. temperaturecooling for 1 hour
9. filtrationThe crystals were collected by filtration
10. washthe obtained crystals were washed with a mixed solution of 2-propanol and n-heptane
11. customdried under reduced pressure