反应详情

温度

65 °C

In flask were placed 7.47 grams (0.019 mole) of 3-(2,3-dichloro-5-nitrophenylmethyl)-1-methyl-6-trifluoromethyluracil and 5.68 grams (0.94 mole) of powdered iron in 115 mL of ethanol and 9 mL of water. Dropwise, 9.0 mL of concentrated hydrochloric acid was added to the reaction mixture. Upon completion of the addition the reaction mixture was heated to 65° C. and maintained at this temperature for three hours. After being cooled to ambient conditions, the reaction mixture was filtered through Celite filter aid, and the collected precipitate was washed several times with ethanol. The solid removed by filtration was then dissolved in ethyl acetate, and this solution was washed twice with a saturated aqueous solution of sodium chloride. The dark brown solution was dried over anhydrous sodium sulfate and filtered. The solvent was evaporated from the filtrate under reduced pressure, leaving 1.62 grams of 3-(5-amino-2,3-dichlorophenylmethyl)-1-methyl-6-trifluoromethyluracil as a solid. This reaction was repeated.

1. customIn flask were placed
2. additionUpon completion of the addition the reaction mixture
3. temperaturemaintained at this temperature for three hours
4. temperatureAfter being cooled to ambient conditions
5. filtrationthe reaction mixture was filtered through Celite
6. filtrationfilter aid
7. washthe collected precipitate was washed several times with ethanol
8. customThe solid removed by filtration
9. dissolutionwas then dissolved in ethyl acetate
10. washthis solution was washed twice with a saturated aqueous solution of sodium chloride
11. dry with materialThe dark brown solution was dried over anhydrous sodium sulfate
12. filtrationfiltered
13. customThe solvent was evaporated from the filtrate under reduced pressure