反应详情

温度

100 °C

Trifluoroacetic acid (2 ml) was added to the compound (102.9 mg, 0.294 mmol) prepared in step 4 and the mixture was stirred in sealed-tube for 20 hours at 100° C. Once the reaction was completed, the reaction mixture was cooled to a room temperature and extracted with dichloromethane. The organic layer was washed with sodium bicarbonate aqueous solution, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was stirred in ethylacetate/hexane/diethylether and the resulting solid was filtered. The filtered solid was washed with diethylether and dried in vacuo to obtain the title compound (57.8 mg, yield: 85.5%, ivory solid).

1. temperaturethe reaction mixture was cooled to a room temperature
2. extractionextracted with dichloromethane
3. washThe organic layer was washed with sodium bicarbonate aqueous solution
4. dry with materialdried over anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. stirringThe residue was stirred in ethylacetate/hexane/diethylether
7. filtrationthe resulting solid was filtered
8. washThe filtered solid was washed with diethylether
9. customdried in vacuo