反应详情

A solution of 23 g of stannous chloride in 20 ml of concentrated hydrochloric acid was added all at once to a solution of 10 g of 3-ethyl-5-(4-methoxyphenyl)-4-(4-nitrophenyl)-4H-1,2,4-triazole in 50 ml of concentrated hydrochloric acid and the mixture was vigorously stirred for 2 hours and was filtered. The recovered product was washed with N hydrochloric acid and was added to aqueous 5N sodium hydroxide solution. The mixture was stirred for 2 hours and was filtered and the white crystals were washed and dried at 110° C. under reduced pressure. The 12.5 g of crystals were dissolved in boiling toluene and the mixture was filtered. The filtrate was iced for 16 hours and was vacuum filtered. The product was dried to obtain 3.8 g of 4-[3-ethyl-5-(4-methoxyphenyl)-4H-1,2,4-triazol-4-yl]-benzeneamine in the form of crystals melting at 216° C.

1. filtrationwas filtered
2. washThe recovered product was washed with N hydrochloric acid
3. additionwas added to aqueous 5N sodium hydroxide solution
4. stirringThe mixture was stirred for 2 hours
5. filtrationwas filtered
6. washthe white crystals were washed
7. customdried at 110° C. under reduced pressure
8. dissolutionThe 12.5 g of crystals were dissolved
9. filtrationthe mixture was filtered
10. waitThe filtrate was iced for 16 hours
11. filtrationfiltered
12. customThe product was dried