Reaktion #5334

Reaktionsgleichung

4'-methylbiphenyl-2-carboxamide

N-bromo-succinimide

AIBN

→

4'-bromomethylbiphenyl-2-carboxamide

Lösungsmittel

benzene

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeResulting crystalline precipitates
2. 2
   Filtrationwere collected by filtration
3. 3
   Waschenwashed with isopropylether
4. 4
   workup.STIRRINGThe suspension was stirred for 30 minutes
5. 5
   Filtrationinsoluble materials were collected by filtration
6. 6
   Sonstigedried
7. 7
   Sonstigeto give crude crystals
8. 8
   SonstigeRecrystallization from ethyl acetate methanol afforded colorless needles (1.6 g, 55%), m.p. 220°-221° C. (decomp.)

Vorschrift

A mixture of 4'-methylbiphenyl-2-carboxamide (2.1 g), N-bromo-succinimide (2.5 g) and azobisisobutyronitrate (AIBN; 82 mg) in benzene (20 ml) was stirred for 20 hours at 60° to 70° C. Resulting crystalline precipitates were collected by filtration, washed with isopropylether and suspended in water. The suspension was stirred for 30 minutes, and insoluble materials were collected by filtration and dried to give crude crystals. Recrystallization from ethyl acetate methanol afforded colorless needles (1.6 g, 55%), m.p. 220°-221° C. (decomp.).

Quelle