HRID2172410

反应详情

EQUATION

反应方程式

HRID 2172410 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Bis(4-bromophenyl)amine (4.0 g, 12.3 mmol) and phenylboronic acid (4.0 g, 32.7 mmol) were mixed in 250 mL of toluene and 60 mL of ethanol. The solution was bubbled with nitrogen while stirring for 15 minutes. Pd(PPh3)4 (1.4 g, 1.23 mmol) and K3PO4 (13.5 g, 64 mmol) were added in sequence. The mixture was heated to reflux overnight under nitrogen. After cooling, the reaction mixture was filtered through filter paper and the solvent was then evaporated. The solid was redissolved in nitrogen-purged hot toluene and was filtered through a Celite®/silica pad when the solution was still hot. The solvent was then evaporated. The white crystalline solid was washed by hexane and air dried to obtain 3.8 g of product.

WORKUP

后处理

  1. customThe solution was bubbled with nitrogen
  2. temperatureThe mixture was heated
  3. temperatureto reflux overnight under nitrogen
  4. temperatureAfter cooling
  5. filtrationthe reaction mixture was filtered
  6. filtrationthrough filter paper
  7. customthe solvent was then evaporated
  8. dissolutionThe solid was redissolved in nitrogen-
  9. custompurged hot toluene
  10. filtrationwas filtered through a Celite®/silica pad when the solution
  11. customThe solvent was then evaporated
  12. washThe white crystalline solid was washed by hexane and air
  13. customdried