تفاعل #63834

معادلة التفاعل

sulfuric acid

2-chloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)benzeneacetonitrile

→

2-chloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)-benzeneacetamide

المردود 54.0%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe product was filtered off
2. 2
   غسيلwashed with water
3. 3
   أخرىpurified by column chromatography over silica gel using
4. 4
   workup.ADDITIONa mixture of trichloromethane and methanol (95:5 by volume) as eluent
5. 5
   أخرىThe pure fractions were collected
6. 6
   أخرىthe eluent was evaporated in vacuo
7. 7
   workup.STIRRINGThe residue was stirred in 2,2'-oxybispropane
8. 8
   ترشيحThe product was filtered off
9. 9
   أخرىdried

الإجراء التجريبي

To 30 parts of a sulfuric acid solution in water (90:10 by volume) were added portionwise during a period of 5 minutes 2 parts of 2-chloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)benzeneacetonitrile at room temperature. Upon completion, stirring was continued for 2 hours at 80° C. The reaction mixture was poured into ice water. The product was filtered off, washed with water and purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated in vacuo. The residue was stirred in 2,2'-oxybispropane. The product was filtered off and dried, yielding 1.1 parts (54%) of 2-chloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)-benzeneacetamide; mp. 160.7° C. (intermediate 26).

المصدر