反应详情

温度

70 °C

8.9 g (39.7 mmol, 4 eq.) of tin(II) chloride dihydrate were added to a solution of 2.7 g (9.9 mmol) of 5-(4-nitrophenyl)-3-(trifluoromethyl)-1H-1,2,4-triazole in 110 ml of ethanol, and the mixture was stirred at 70° C. for 1 h. The reaction mixture was poured into ice-water, and sodium bicarbonate was added carefully until a pH of 8 had been reached. The mixture was filtered through a filter layer and the residue was washed with ethyl acetate. After phase separation, the aqueous phase was washed twice with ethyl acetate. The combined organic phases were washed with aqueous sodium chloride solution, dried (magnesium sulphate), filtered and concentrated under reduced pressure. Yield: 1.9 g (79% of theory)

1. additionwas added carefully until a pH of 8
2. filtrationThe mixture was filtered through a filter layer
3. washthe residue was washed with ethyl acetate
4. customAfter phase separation
5. washthe aqueous phase was washed twice with ethyl acetate
6. washThe combined organic phases were washed with aqueous sodium chloride solution
7. dry with materialdried (magnesium sulphate)
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure