反应详情

温度

0 °C

The compound obtained in (1) above 73 gm was dissolved into 600 ml of acetic acid. To the solution were added 20 ml of 40% perchloric acid and 10% palladium-on-carbon to effect catalytic hydrogenation under 5 atm. After the evaporation of acetic acid and the addition of 100 ml of water, the residue was extracted with ethyl acetate. The extract was washed with saturated sodium bicarbonate and saturated brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated and 100 ml of dichloromethane, 74 gm of sodium carbonate, and 30 ml of thionyl chloride were added to the residue. The mixture was heated under reflux for 3 hours and then cooled to 0° C., and 150 ml of methanol was slowly added, followed by stirring for 12 hours at room temperature. After the addition of 300 ml of ethyl acetate, the resulting product was washed with water and saturated brine in this order, and dried over anhydrous sodium sulfate. The solvent was evaporated to obtain 66.7 gm of the title compound.

1. customAfter the evaporation of acetic acid
2. additionthe addition of 100 ml of water
3. extractionthe residue was extracted with ethyl acetate
4. washThe extract was washed with saturated sodium bicarbonate and saturated brine in this order
5. dry with materialdried over anhydrous sodium sulfate
6. customThe solvent was evaporated
7. addition100 ml of dichloromethane, 74 gm of sodium carbonate, and 30 ml of thionyl chloride were added to the residue
8. temperatureThe mixture was heated
9. temperatureunder reflux for 3 hours
10. addition150 ml of methanol was slowly added
11. additionAfter the addition of 300 ml of ethyl acetate
12. washthe resulting product was washed with water and saturated brine in this order
13. dry with materialdried over anhydrous sodium sulfate
14. customThe solvent was evaporated