反应详情

8.45 g of ethyl 5-amino-1-t-butyl-1H-pyrazole-4-carboxylate was dissolved in 60 ml of acetic acid, and 7.93 g of 2,5-dimethoxytetrahydrofuran was then added. The mixture was heated to reflux for 2 hours. The reaction mixture was concentrated under reduced pressure. After water was added, the residue was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 8.95 g of ethyl 5-(1H-pyrrol-1-yl)-1-t-butyl-1H-pyrazole-4-carboxylate.

1. temperatureThe mixture was heated
2. temperatureto reflux for 2 hours
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. additionAfter water was added
5. extractionthe residue was extracted with ethyl acetate
6. washThe organic layer was washed with water
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure