反应详情

温度

90 °C

3-chloro-1-(3,4-diethylphenyl)-1-propanone (15.5 g) is dissolved in 66 mL concentrated sulphuric acid and heated to 90° C. for 4 hours. The reaction mixture is cooled, ice (70 g) is added, and the aqueous solution extracted twice with toluene. The organic layer is washed with sodium bicarbonate, saturated aqueous NaCl, and treated with activated charcoal and magnesium suphate. After filtration, the solvent is removed in vacuo. The product is purified by flash column chromatography (silica, hexane/ethylacetate 10:1), and further crystallised in hexane.

1. temperatureThe reaction mixture is cooled
2. extractionthe aqueous solution extracted twice with toluene
3. washThe organic layer is washed with sodium bicarbonate, saturated aqueous NaCl
4. additiontreated with activated charcoal and magnesium suphate
5. filtrationAfter filtration
6. customthe solvent is removed in vacuo
7. customThe product is purified by flash column chromatography (silica, hexane/ethylacetate 10:1)
8. customfurther crystallised in hexane