反应详情

温度

80 °C

In a 250 ml three-necked round-bottomed flask, 4.00 g 4-chloro-3-trifluoromethyl-phenol is dissolved in 80 ml of dry methyl-ethyl-ketone. 3.85 g potassium carbonate followed by 4.70 g of 3-bromo-2-chloro-4-methyl-5-nitro-pyridine are added. The resulting brown suspension is heated to 80° C. under stirring for 3 hours. Afterwards, the green suspension is allowed to reach an ambient temperature and it then poured into water. The mixture is extracted with ethyl actetate (3×50 ml). The combined organic phases are washed with brine, dried over sodium sulfate, filtered and the solvent removed in vacuo. After purification of the raw product on silica gel with cyclohexane/ethyl actetae 19:1 (v:v) 7.36 g of the title compound are obtained as a light yellow gum that solidifies upon standing (MP: 73-74° C.).

1. additionare added
2. customto reach an ambient temperature
3. extractionThe mixture is extracted with ethyl actetate (3×50 ml)
4. washThe combined organic phases are washed with brine
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. customthe solvent removed in vacuo
8. customAfter purification of the raw product on silica gel with cyclohexane/ethyl actetae 19:1 (v:v) 7.36 g of the title compound
9. customare obtained as a light yellow gum