反应 #2171036

ord-51c4fc4537f64441b3ecb7489f8b3016

反应方程式

Nc1c(F)cc(Br)cc1F
4-bromo-2,6-difluoroaniline
BrCc1ccccc1
benzyl bromide
O=C([O-])[O-].[K+].[K+]
potassium carbonate
Fc1cc(Br)cc(F)c1N(Cc1ccccc1)Cc1ccccc1
dibenzyl(4-bromo-2,6-difluorophenyl)amine
收率 85.6%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度is refluxed for 48 hours
  2. 2
    其他The mixture is subsequently evaporated in a rotary evaporator
  3. 3
    workup.DISSOLUTIONthe residue is dissolved in toluene
  4. 4
    萃取extracted with hydrochloric acid (10%)
  5. 5
    其他the toluene phase is evaporated in a rotary evaporator
  6. 6
    workup.STIRRINGstirred with silica gel for about 4.5 hours
  7. 7
    过滤filtered with suction
  8. 8
    其他evaporated in a rotary evaporator

实验过程

A suspension of 416 g of 4-bromo-2,6-difluoroaniline, 752 g of benzyl bromide and 608 g of potassium carbonate in 2 l of acetonitrile is refluxed for 48 hours. The mixture is subsequently evaporated in a rotary evaporator, the residue is dissolved in toluene and extracted with hydrochloric acid (10%), the toluene phase is evaporated in a rotary evaporator, and the product is stirred into heptane and stirred with silica gel for about 4.5 hours, filtered with suction and evaporated in a rotary evaporator, giving dibenzyl(4-bromo-2,6-difluorophenyl)amine, yield 85.6%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06716491B2uspto-grants-2004_04