反应详情

The product from Step 2 (4 g) and sodium acetate (6 g) were refluxed together in glacial acetic acid (60 ml) for 1 hour. The mixture was cooled, diluted with ethyl acetate (300 ml) and washed with water (3×100 ml), then with aqueous sodium bicarbonate and again with water, dried and evaporated down. The residue was chromatographed on a column of silica gel eluting with a 1:9 mixture of ethyl acetate-hexane to afford, after trituration in ether and filtration, the pure title compound (1.2 g), m.p. 195°-196° C.

1. temperatureThe mixture was cooled
2. washwashed with water (3×100 ml)
3. dry with materialwith aqueous sodium bicarbonate and again with water, dried
4. customevaporated down
5. customThe residue was chromatographed on a column of silica gel eluting with a 1:9 mixture of ethyl acetate-hexane
6. customto afford
7. filtrationafter trituration in ether and filtration