反应详情

温度

60 °C

A 50 ml two-necked round-bottomed flask equipped with a magnetic bar, a thermometer and a reflux condenser is charged with DMF (50 ml), 3-tert-butyl-phenol (1.5 g), 2-chloro-3-methyl-5-nitro-pyridine (1.73 g) and potassium carbonate (2.76 g). The reaction mixture is heated at 60° C. for 2 hours. After cooling the mixture to room temperature it is then poured into water (200 ml). The mixture is then extracted with ethylacetate (2×40 ml). The combined organic layers are dried over sodium sulfate, filtered and the solvent is removed in vacuo. Purification of this crude material by flash chromatography over silica gel with hexane/ethyl acetate 4:1 (v:v) gives 2.55 g of the compound as a yellow oil.

1. customA 50 ml two-necked round-bottomed flask equipped with a magnetic bar
2. temperatureAfter cooling the mixture to room temperature it
3. extractionThe mixture is then extracted with ethylacetate (2×40 ml)
4. dry with materialThe combined organic layers are dried over sodium sulfate
5. filtrationfiltered
6. customthe solvent is removed in vacuo
7. customPurification of this crude material by flash chromatography over silica gel with hexane/ethyl acetate 4:1 (v:v)