反应详情

A 100 mL EtOH solution of 1.0 g (2.1 mmol) 8-(3-nitrobenzyl)-4-(cyclohexylamino)-1-(3-fluorophenyl)-1,3,8-triazaspiro[4.5]dec-3-en-2-one (example 104) and 0.57 g (2.5 mmol) SnCl2 dihydrate was heated to reflux and allowed to stir overnight. HPLC/MS showed complete conversion so the reaction mixture was filtered through celite washed with EtOH then the filtrate was concentrated. The remaining oil was partitioned between 3N NaOH and EtOAc. A thick white precipitate formed in the aqueous layer. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated to pure product.

1. temperatureto reflux
2. filtrationwas filtered through celite
3. washwashed with EtOH
4. concentrationthe filtrate was concentrated
5. customThe remaining oil was partitioned between 3N NaOH and EtOAc
6. customA thick white precipitate formed in the aqueous layer
7. washThe organic layer was washed with brine
8. dry with materialdried over Na2SO4
9. filtrationfiltered
10. concentrationconcentrated to pure product