反应详情

A solution of 2-acetylpyridine (5.0 g, 40 mmol) and diethyl oxalate (5.9 g, 40 mmol) in diethylether (75 ml) was cooled to 0° C. and treated with sodium ethylate (16.6 ml, 21% solution in ethanol). While stirring overnight, the reaction mixture was allowed to warm-up slowly to ambient temperature. The reaction mixture was acidified with acetic acid, diluted with water and extracted with diethylether. The combined organic phases were washed with water and brine, dried and evaporated. The isolated residue was triturated with heptane (30 ml) and diethylether (5 ml) for 2 h and the resulting suspension was filtrated to collect the product. This process was repeated to obtain the product as light brown solid (3.96 g, 44%). MS: M=220.1 (M−H)−

1. extractionextracted with diethylether
2. washThe combined organic phases were washed with water and brine
3. customdried
4. customevaporated
5. customThe isolated residue was triturated with heptane (30 ml) and diethylether (5 ml) for 2 h
6. filtrationthe resulting suspension was filtrated
7. customto collect the product