反应详情

温度

75 °C

156.9 g (2.4 mol) of zinc, 500 ml of ethanol and then 77 g (0.3 mol) of 4-fluoro-6-methyl-3-nitrobenzenesulfonyl chloride were placed in a 2-liter eggplant-shaped flask equipped with a mechanical stirrer, a thermometer and a dropping funnel. Thereinto was dropped 500 g (5 mol) of hydrochloric acid in a water bath so that the temperature of the reaction system did not exceed 50° C., followed by stirring at 75° C. for 6 hours. Ethanol was distilled off under reduced pressure; the residue was cooled to room temperature; sodium bicarbonate was added to neutralize the reaction system; extraction was conducted twice with ethyl acetate; the ethyl acetate layer was washed with water and then with a saturated aqueous sodium chloride solution. The ethyl acetate layer was dried with anhydrous sodium sulfate and subjected to distillation under reduced pressure to distil off ethyl acetate to obtain 41 g of a title compound at a yield of 87%.

1. customequipped with a mechanical stirrer
2. customdid not exceed 50° C.
3. distillationEthanol was distilled off under reduced pressure
4. temperaturethe residue was cooled to room temperature
5. additionsodium bicarbonate was added
6. extractionextraction
7. washthe ethyl acetate layer was washed with water
8. dry with materialThe ethyl acetate layer was dried with anhydrous sodium sulfate
9. distillationsubjected to distillation under reduced pressure
10. customto distil off ethyl acetate