反应详情

温度

5 °C

1.6 ml of fuming nitric acid were added, over the course of 20 minutes, to a solution of 4.1 g of 1-(2-hydroxyphenyl)-2-methylpropan-1-one in 25 ml of acetic acid cooled to 5° C. The reaction medium was stirred at ambient temperature for 5 hours (followed by TLC, 10/1 heptane/ethyl acetate). The reaction was stopped before all the 1-(2-hydroxyphenyl)-2-methylpropan-1-one was consumed. The reaction medium was diluted with 70 ml of water and then extracted with ethyl acetate (4:1, 3×50 ml). The organic phases were combined, washed with water (20 ml) and then with a saturated sodium chloride solution (25 ml), and dried over magnesium sulfate. The solvent was evaporated off and the residue was chromatographed on silica. 1.40 g of 1-(2-hydroxy-5-nitrophenyl)-2-methylpropan-1-one and 1.2 g of 1-(2-hydroxy-3-nitrophenyl)-2-methylpropan-1-one were obtained.

1. customwas consumed
2. additionThe reaction medium was diluted with 70 ml of water
3. extractionextracted with ethyl acetate (4:1, 3×50 ml)
4. washwashed with water (20 ml)
5. dry with materialwith a saturated sodium chloride solution (25 ml), and dried over magnesium sulfate
6. customThe solvent was evaporated off
7. customthe residue was chromatographed on silica