HRID5238

反应详情

EQUATION

反应方程式

HRID 5238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

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.).

WORKUP

后处理

  1. customResulting crystalline precipitates
  2. filtrationwere collected by filtration
  3. washwashed with isopropylether
  4. stirringThe suspension was stirred for 30 minutes
  5. filtrationinsoluble materials were collected by filtration
  6. customdried
  7. customto give crude crystals
  8. customRecrystallization from ethyl acetate methanol afforded colorless needles (1.6 g, 55%), m.p. 220°-221° C. (decomp.)