反应详情

Titanium tetrachloride (1.99 g) was slowly added to a mixture of (5-amino-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid ethyl ester (3.48 g), benzophenone (2.81 g) and DABCO (4.72 g) in chlorobenzene (112 ml). Resulting mixture was heated to reflux for 2.5 h. After cooling, reaction mixture was filtered through a pad of celite and rinsed with ethyl acetate. Filtrate was concentrated and the residue was purified by silica gel chromatography (25%-40% ethyl acetate in hexanes) to give the title compound (3.03 g). MS-(+)-ion: M+1=413.3.

1. customResulting mixture
2. temperaturewas heated
3. temperatureto reflux for 2.5 h
4. temperatureAfter cooling
5. customreaction mixture
6. filtrationwas filtered through a pad of celite
7. washrinsed with ethyl acetate
8. concentrationFiltrate was concentrated
9. customthe residue was purified by silica gel chromatography (25%-40% ethyl acetate in hexanes)