反应详情

Ethyl [4-(4,9-diethoxy-1,3-dioxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetate (339, 73 mmol) and zinc (909, 1.38 mol) were refluxed in acetic acid for 66 h. An additional quantity of zinc (25 g, 0.38 mol) was added and reflux continued for 18 h. The mixture was filtered hot and the filtrate was evaporated to a yellow solid. The solid was purified by 800 g Biotage column eluting with 20% ethyl acetate/hexane to give a white solid, which was triturated in ether to give a white solid. A further fraction was obtained by crystallisation from the ether residues. A total of 10.2 g, 32% of ethyl [4-(4,9-diethoxy-1-oxo-1,3-dihydro-2H-benzo[f]isoindol-2-yl)phenyl]acetate was obtained.

1. temperaturereflux
2. filtrationThe mixture was filtered hot
3. customthe filtrate was evaporated to a yellow solid
4. customThe solid was purified by 800 g Biotage column
5. washeluting with 20% ethyl acetate/hexane
6. customto give a white solid, which
7. customwas triturated in ether
8. customto give a white solid