反応 #5334

反応方程式

4'-methylbiphenyl-2-carboxamide

N-bromo-succinimide

AIBN

→

4'-bromomethylbiphenyl-2-carboxamide

溶媒

benzene

反応条件

後処理

1. 1
   その他Resulting crystalline precipitates
2. 2
   ろ過were collected by filtration
3. 3
   洗浄washed with isopropylether
4. 4
   workup.STIRRINGThe suspension was stirred for 30 minutes
5. 5
   ろ過insoluble materials were collected by filtration
6. 6
   その他dried
7. 7
   その他to give crude crystals
8. 8
   その他Recrystallization from ethyl acetate methanol afforded colorless needles (1.6 g, 55%), m.p. 220°-221° C. (decomp.)

実験手順

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.).

出典