反应详情

温度

50 °C

A mixture of 4.88 g of 2-chloro3-nitro-5-(trifluoromethyl)pyridine, 1.81 g of thiourea and 40 ml of ethanol was stirred at 50° C. for 5.5 hours. The reaction mixture was cooled down to room temperature, then, concentrated under reduced pressure. To the residue was added 24 ml of water and a mixture of 2.8 g of sodium hydroxide and 6 ml of water, and this was stirred at room temperature for 1.5 hours. The reaction mixture was washed with diethyl ether, then, acetic acid was added. This was cooled with ice, and the deposited solid was collected by filtration. This solid was dried under reduced pressure, to obtain 3.84 g of 3-nitro-5-(trifluoromethyl)pyridine-2-thiol.

1. temperatureThe reaction mixture was cooled down to room temperature
2. concentrationconcentrated under reduced pressure
3. additionTo the residue was added 24 ml of water
4. additiona mixture of 2.8 g of sodium hydroxide and 6 ml of water
5. stirringthis was stirred at room temperature for 1.5 hours
6. washThe reaction mixture was washed with diethyl ether
7. additionacetic acid was added
8. temperatureThis was cooled with ice
9. filtrationthe deposited solid was collected by filtration
10. customThis solid was dried under reduced pressure