HRID2206835

反应详情

EQUATION

反应方程式

HRID 2206835 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of N-phenylnaphthalen-1-amine (4.41 g, 20 mmol), 4,4′-dibromo-1,1′-biphenyl (15 g, 48 mmol), sodium tert-butoxide (4.8 g, 50 mmol) and Pd(dppf)Cl2 (0.44 g, 0.6 mmol) in anhydrous toluene (100 ml) was degassed and heated at 80° C. for 10 hours. After cooling to RT, the mixture was poured into dichloromethane (400 ml) and stirred for 30 min, then washed with brine (100 ml). The organic is collected and dried over Na2SO4, loaded on silica gel, and purified by flash column (hexanes to hexanes/ethyl acetate 90:1) to give a solid which was washed with methanol and dried under air to give a white solid 4 (5.58 g, in 62% yield).

WORKUP

后处理

  1. customwas degassed
  2. temperatureAfter cooling to RT
  3. additionthe mixture was poured into dichloromethane (400 ml)
  4. washwashed with brine (100 ml)
  5. customThe organic is collected
  6. dry with materialdried over Na2SO4
  7. custompurified by flash column (hexanes to hexanes/ethyl acetate 90:1)
  8. customto give a solid which
  9. washwas washed with methanol
  10. customdried under air