반응 #63843

반응 방정식

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

수율 67.2%

용매

acetic acid

반응 조건

후처리

1. 1
   workup.STIRRINGStirring
2. 2
   온도at reflux temperature
3. 3
   여과The zinc salts were filtered off
4. 4
   기타the filtrate was evaporated
5. 5
   세척The residue was washed with water whereupon the solid product
6. 6
   여과was filtered off
7. 7
   workup.DISSOLUTIONdissolved in a mixture of trichlorometmhane and methanol (90:10 by volume)
8. 8
   기타The solution was dried
9. 9
   여과filtered
10. 10
    기타evaporated
11. 11
    세척The residue was washed with ethyl acetate and 2,2'-oxybispropane
12. 12
    기타dried

실험 절차

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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