反应详情

A mixture of 6.85 g (43.3 mmol) of ethyl isobutyrylacetate, 10.69 g (56.3 mmol) of 2-amino-4'-fluoracetophenone hydrochloride, 16.3 ml of acetic acid, 6.04 g of sodium acetate, and 10.8 ml of water is refluxed for 4 hours. After cooling, the reaction mixture is adjusted to pH 8 with saturated NaHCO3 and extracted with ether. The extract, 8.36 g, is subjected to column chromatography with silica gel, eluting with methylene chloride to give 6.12 g (Yield:51.3%) of the compound 1.

1. temperatureis refluxed for 4 hours
2. temperatureAfter cooling
3. extractionextracted with ether
4. washeluting with methylene chloride