反应详情

A three-necked round-bottom flask equipped with condenser, mechanical stirrer, thermometer, is loaded with N,N-diisopropyl-3-phenyl-3-hydroxy-propionamide (1.0 g; 0.0041 mol), p-cresol (0.48 g; 0.0044 mol) and polyphosphoric acid (16.5 g). After five hours under stirring at room temperature the reaction is completed. The reaction mixture is poured in ice/water (10 g), alkalinized to pH 9-10 with NaOH 50% w/w and left under stirring for 30 minutes, then diluted with toluene (30 ml). The phases are separated and the aqueous phase is extracted with toluene (2×30 ml). The combined organic phases are dried over sodium sulfate and evaporated to dryness. The resulting oil is purified by flash chromatography (hexane/ethyl acetate 7:3). 0.48 g of product, as a pale yellow oil, are obtained.

1. customA three-necked round-bottom flask equipped with condenser, mechanical stirrer
2. waitleft
3. stirringunder stirring for 30 minutes
4. customThe phases are separated
5. extractionthe aqueous phase is extracted with toluene (2×30 ml)
6. dry with materialThe combined organic phases are dried over sodium sulfate
7. customevaporated to dryness
8. customThe resulting oil is purified by flash chromatography (hexane/ethyl acetate 7:3)