反应详情

A solution of 4a (100 mg) in pyridine (5 ml) was added acetic anhydride (2 ml). The mixture was heated at 110° for 1 hour and concentrated in vacuo. The crude mixture was purified via preparative tlc using 2000 μm silica gel plates developed with 30% ethyl acetate in chloroform. The isolated product was recrystallized from acetone-hexane to give pure Z methyl 1-[4-(N-acetylaminosulfonyl)phenyl]methylene-5-methoxy-2-methyl-1H-3-indenylacetate (55 mg, 50%): m.p. 172.5°-174.5° C.

1. temperatureThe mixture was heated at 110° for 1 hour
2. concentrationconcentrated in vacuo
3. customThe crude mixture was purified via preparative tlc
4. customThe isolated product was recrystallized from acetone-hexane