反応 #630055

反応方程式

3-ethyl-5-(4-methoxyphenyl)-4-(4-nitrophenyl)-4H-1,2,4-triazole

→

4-[3-ethyl-5-(4-methoxyphenyl)-4H-1,2,4-triazol-4-yl]-benzeneamine

収率 41.9%

溶媒

hydrochloric acid

hydrochloric acid

反応条件

後処理

1. 1
   ろ過was filtered
2. 2
   洗浄The recovered product was washed with N hydrochloric acid
3. 3
   workup.ADDITIONwas added to aqueous 5N sodium hydroxide solution
4. 4
   workup.STIRRINGThe mixture was stirred for 2 hours
5. 5
   ろ過was filtered
6. 6
   洗浄the white crystals were washed
7. 7
   その他dried at 110° C. under reduced pressure
8. 8
   workup.DISSOLUTIONThe 12.5 g of crystals were dissolved
9. 9
   ろ過the mixture was filtered
10. 10
    workup.WAITThe filtrate was iced for 16 hours
11. 11
    ろ過filtered
12. 12
    その他The product was dried

実験手順

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.

出典