HRID2275937

反应详情

EQUATION

反应方程式

HRID 2275937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

17.5 g (40.18 mmol) of 10-biphenyl-4-yl-12,12-dimethyl-10,12-dihydro-10-azaindeno[2,1-b]fluorene are suspended in 450 ml of acetonitrile, and 7.15 g (40.18 mmol) of N-bromosuccinimide are added in portions at −20° C. at such a rate that the reaction temperature does not rise above −20° C. The mixture is stirred for a further 18 h, during which the temperature is allowed to come to RT. The reaction mixture is subsequently evaporated in a rotary evaporator, dissolved in dichloromethane and washed with water. The residue is dried, evaporated and subsequently recrystallised from toluene to a purity of 99.3%, giving 10.9 g (53%) of the product as a white solid.

WORKUP

后处理

  1. customdoes not rise above −20° C
  2. customto come to RT
  3. customThe reaction mixture is subsequently evaporated in a rotary evaporator
  4. dissolutiondissolved in dichloromethane
  5. washwashed with water
  6. customThe residue is dried
  7. customevaporated
  8. customsubsequently recrystallised from toluene to a purity of 99.3%