反应详情

A 250 ml two-necked round-bottomed flask equipped with a magnetic bar, a thermometer and a reflux condenser is charged with DMF (30 ml), 4-chloro-3-trifluoromethyl-phenol (4.5 g), 2-chloro-4-methyl-5-nitro-pyridine (4.0 g) and potassium carbonate (6.4 g). The reaction mixture is stirred at ambient temperature for 1 hour, poured into water (300 ml), acidified with HCl 5 molar (15 ml) and then extracted with ethylacetate (4×50 ml). The combined organic layers are washed with brine (100 ml), dried over sodium sulfate, filtered and the solvent is removed in vacuo. Purification by flash chromatography over silica gel with hexane/ethyl acetate 7:3 (v:v) gives 7.03 g of the compound as a red solid (MP: 75-80° C.).

1. customA 250 ml two-necked round-bottomed flask equipped with a magnetic bar
2. extractionextracted with ethylacetate (4×50 ml)
3. washThe combined organic layers are washed with brine (100 ml)
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customthe solvent is removed in vacuo
7. customPurification by flash chromatography over silica gel with hexane/ethyl acetate 7:3 (v:v)