HRID1269587

反应详情

EQUATION

反应方程式

HRID 1269587 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

Palladium (II) acetate (5.4 mg, 0.024 mmol) and (S)-2,2′-bis(diphenylphosphino)-1,1′-binapthyl (22 mg, 0.036 mmol) in anhydrous toluene (1.2 mL) were stirred together at 70° C. in a sealed reactivial for 30 minutes. The vial was then allowed to attain room temperature before the methyl {4-[(butylamino)methyl]-2-methylphenoxy}acetate (96 mg, 0.36 mmol), 2-bromo-6-[4-(trifluoromethyl)phenyl]pyridine (90.6 mg, 0.3 mmol) and caesium carbonate (137 mg, 0.42 mmol) were added. The vial was then sealed and heated at 80° C. for 18 h. The reaction mixture was allowed to cool to room temperature, the reaction mixture filtered and the solvent removed in vacuo. Purification by SPE (Silica, 10 g) eluting 99:1–50:1 cyclohexane:EtOAc afforded the title compound as a colourless oil (50 mg).

WORKUP

后处理

  1. additionwere added
  2. customThe vial was then sealed
  3. temperatureto cool to room temperature
  4. filtrationthe reaction mixture filtered
  5. customthe solvent removed in vacuo
  6. customPurification by SPE (Silica, 10 g)
  7. washeluting 99:1–50:1 cyclohexane