Реакция #63843

Уравнение реакции

2,6-dichloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin2(3H)-yl)benzeneacetic acid

→

2,6-dichloro-α-(4-chlorophenyl)-4-(3,4,5,6-tetrahydro-3,5-dioxo-1,2,4-triazin-2(1H)-yl)benzeneacetic acid

Выход 67.2%

Растворители

acetic acid

Условия реакции

Обработка

1. 1
   workup.STIRRINGStirring
2. 2
   Температураat reflux temperature
3. 3
   ФильтрацияThe zinc salts were filtered off
4. 4
   Другоеthe filtrate was evaporated
5. 5
   ПромывкаThe residue was washed with water whereupon the solid product
6. 6
   Фильтрацияwas filtered off
7. 7
   workup.DISSOLUTIONdissolved in a mixture of trichlorometmhane and methanol (90:10 by volume)
8. 8
   ДругоеThe solution was dried
9. 9
   Фильтрацияfiltered
10. 10
    Другоеevaporated
11. 11
    ПромывкаThe residue was washed with ethyl acetate and 2,2'-oxybispropane
12. 12
    Другоеdried

Методика

To a stirred and refluxed solution of 1.5 parts of 2,6-dichloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin2(3H)-yl)benzeneacetic acid in 100 parts of acetic acid were added 3 parts of zinc. Stirring was continued for 30 minutes at reflux temperature. The zinc salts were filtered off and the filtrate was evaporated. The residue was washed with water whereupon the solid product was filtered off and dissolved in a mixture of trichlorometmhane and methanol (90:10 by volume). The solution was dried, filtered and evaporated. The residue was washed with ethyl acetate and 2,2'-oxybispropane and dried, yielding 0.98 parts (67.2%) of 2,6-dichloro-α-(4-chlorophenyl)-4-(3,4,5,6-tetrahydro-3,5-dioxo-1,2,4-triazin-2(1H)-yl)benzeneacetic acid; mp. 194.2° C. (compound 1).

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