반응 #5334

ord-38557339d9a449aeba84ca978a2ba6b2

반응 방정식

Cc1ccc(-c2ccccc2C(N)=O)cc1
4'-methylbiphenyl-2-carboxamide
O=C1CCC(=O)N1Br
N-bromo-succinimide
CC(C)(C#N)N=NC(C)(C)C#N
AIBN
NC(=O)c1ccccc1-c1ccc(CBr)cc1
4'-bromomethylbiphenyl-2-carboxamide

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Resulting crystalline precipitates
  2. 2
    여과were collected by filtration
  3. 3
    세척washed with isopropylether
  4. 4
    workup.STIRRINGThe suspension was stirred for 30 minutes
  5. 5
    여과insoluble materials were collected by filtration
  6. 6
    기타dried
  7. 7
    기타to give crude crystals
  8. 8
    기타Recrystallization from ethyl acetate methanol afforded colorless needles (1.6 g, 55%), m.p. 220°-221° C. (decomp.)

실험 절차

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.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05243054uspto-grants-1993_09