HRID1375221

反应详情

EQUATION

反应方程式

HRID 1375221 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 17.89 g (44.0 mmol) 4-(tert-butyl-diphenyl-silanyloxy)-3-methoxy-phenyl-boronic acid, 6.89 g (31.45 mmol) 2-iodoaniline, 17.4 g (125.8 mmol) K2CO3 and 425 mg (6 mol %) Pd(OAc)2 in 140 ml THF and 80 ml H2O is heated to reflux for 20 hours. After cooling the mixture is filtrated over cellite and concentrated. The residue is dissolved in ethyl acetate and washed with water. After drying (MgSO4) and evaporating the solvent, the residue is subjected to flash-chromatography (ethyl acetate/hexane 1:9). Yield: 4′-(tert-Butyl-diphenyl-silanyloxy)-3′-methoxy-biphenyl-2-ylamine is isolated as a colorless oil.

WORKUP

后处理

  1. temperatureto reflux for 20 hours
  2. temperatureAfter cooling the mixture
  3. filtrationis filtrated over cellite
  4. concentrationconcentrated
  5. dissolutionThe residue is dissolved in ethyl acetate
  6. washwashed with water
  7. dry with materialAfter drying (MgSO4)
  8. customevaporating the solvent