反应详情

To a 1 L round-bottomed flask equipped with Dean-Stark trap, condenser, and nitrogen inlet were added 21.3 g (123 mmol) 2-amino-6-bromopyridine, 400 mL toluene, 14.1 g (123 mmol) acetonylacetone, and 20 drops acetic acid. The reaction was refluxed 5 days (tlc in 1/1:ethyl acetate/hexane, Rf=0.8(product), 0.5 (starting material)), cooled, poured into ethyl acetate, washed with saturated aqueous sodium bicarbonate solution and brine, dried over sodium sulfate, and evaporated. The residue was chromatographed on silica gel using 5% methanol in methylene chloride to afford 14.4 g(47%) of the product as a low-melting yellow solid.

1. customTo a 1 L round-bottomed flask equipped with Dean-Stark trap, condenser, and nitrogen inlet
2. temperaturecooled
3. washwashed with saturated aqueous sodium bicarbonate solution and brine
4. dry with materialdried over sodium sulfate
5. customevaporated
6. customThe residue was chromatographed on silica gel using 5% methanol in methylene chloride