反应详情

A 500-mL Parr reactor bottle was purged with nitrogen and charged with 10% palladium on carbon (50% wet, 2.0 g dry weight), 103c (4.5 g, 18 mmol), 12% hydrochloric acid (9.2 mL, 37 mmol), ethyl acetate (80 mL) and ethanol (52 mL). The bottle was attached to a Parr hydrogenator, evacuated, charged with hydrogen gas to a pressure of 50 psi and shaken for 6 h. After this time, the hydrogen was evacuated, and nitrogen was charged into the bottle. Diatomaceous earth filtration agent (Celite® 521, 10.0 g) was added, and the mixture was filtered through a pad of Celite 521. The filter cake was washed with ethanol (2×50 mL), and the combined filtrates were concentrated to dryness under reduced pressure. The crude residue 103d was carried onto the next step without further purification.

1. customA 500-mL Parr reactor bottle was purged with nitrogen
2. customevacuated
3. additioncharged with hydrogen gas to a pressure of 50 psi
4. customAfter this time, the hydrogen was evacuated
5. additionnitrogen was charged into the bottle
6. filtrationDiatomaceous earth filtration agent (Celite® 521, 10.0 g)
7. additionwas added
8. filtrationthe mixture was filtered through a pad of Celite 521
9. washThe filter cake was washed with ethanol (2×50 mL)
10. concentrationthe combined filtrates were concentrated to dryness under reduced pressure
11. customThe crude residue 103d was carried onto the next step without further purification