反应 #5334

ord-38557339d9a449aeba84ca978a2ba6b2

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05243054uspto-grants-1993_09