تفاعل #4694

معادلة التفاعل

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

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

المردود 41.9%

المذيبات

hydrochloric acid

hydrochloric acid

ظروف التفاعل

المعالجة

1. 1
   ترشيحwas filtered
2. 2
   غسيلThe 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
   ترشيحwas filtered
6. 6
   غسيلthe white crystals were washed
7. 7
   أخرىdried at 110° C. under reduced pressure
8. 8
   workup.DISSOLUTIONThe 12.5 g of crystals were dissolved
9. 9
   ترشيحthe mixture was filtered
10. 10
    workup.WAITThe filtrate was iced for 16 hours
11. 11
    ترشيحfiltered
12. 12
    أخرىThe product was dried

الإجراء التجريبي

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.

المصدر