反应详情

Trifluoroacetic acid (4 mL, 53.8 mmol) was added to a solution of benzyl 3-methyl-2-oxo-1-{[2-(trimethylsilyl)ethoxy]methyl}-2,2′,3,3′-tetrahydro-1H,1′H-spiro[1,8-naphthyridine-4,4′-pyridine]-1′-carboxylate (0.10 g, 0.20 mmol) in dichloromethane (2 mL). After 2 h, the reaction mixture was concentrated. The concentrated mixture was diluted in dichloromethane (2 mL) and ethane-1,2-diamine (4 mL) was added. After 1 h, the reaction mixture was concentrated and saturated aqueous sodium bicarbonate was added. The mixture was extracted with dichloromethane (3×). The combined organic extracts were dried over magnesium sulfate, filtered and concentrated. MS 364.1 (M+1).

1. concentrationthe reaction mixture was concentrated
2. additionThe concentrated mixture was diluted in dichloromethane (2 mL)
3. additionethane-1,2-diamine (4 mL) was added
4. waitAfter 1 h
5. concentrationthe reaction mixture was concentrated
6. additionsaturated aqueous sodium bicarbonate was added
7. extractionThe mixture was extracted with dichloromethane (3×)
8. dry with materialThe combined organic extracts were dried over magnesium sulfate
9. filtrationfiltered
10. concentrationconcentrated