反应详情

温度

110 °C

A mixture of the title compound of Example 78 (100 mg, 0.2 mmol), potassium bis(trimethylsilyl)amide (210 mg, 1.1 mmol) in pyridine-2-methanol (1 ml) was heated to 110° C. for 18 hours. The cooled mixture was partitioned between ethyl acetate (10 ml) and water (10 ml), and the phases separated. The aqueous layer was extracted with ethyl acetate (2×5 ml) and dichloromethane (10 ml), the combined organic solutions dried (Na2SO4) and evaporated under reduced pressure. The residue was purified by column chromatography on silica gel, using methanol:ethyl acetate (10:90) as eluant, and triturated with ether, to afford the title compound (49 mg, 43%) as a solid.

1. customThe cooled mixture was partitioned between ethyl acetate (10 ml) and water (10 ml)
2. customthe phases separated
3. extractionThe aqueous layer was extracted with ethyl acetate (2×5 ml) and dichloromethane (10 ml)
4. dry with materialthe combined organic solutions dried (Na2SO4)
5. customevaporated under reduced pressure
6. customThe residue was purified by column chromatography on silica gel
7. customtriturated with ether