HRID383852

反应详情

EQUATION

反应方程式

HRID 383852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

7-Bromo-5-methoxy-N,N-dimethylbenzofuran-2-carboxamide (0.20 g, 0.67 mmol), 1-(2-pyridin-2-yl-ethyl)piperazine (0.13 g, 0.67 mmol), Pd2 dba3 (0.031 g, 0.030 mmol), 2-dicyclohexylphosphino-2′,4′,6′-tri-iso-propyl-1,1′-biphenyl (0.032 g, 0.070 mmol) and sodium t-butoxide (0.14 g, 1.41 mmol) were heated in toluene (1 mL) at 100° C. for 2 h. The mixture was allowed to cool. Ethyl acetate was added and the mixture was filtered through a pad of Celite. The filtrate was washed with water and brine, dried over MgSO4 and the solvent was removed by rotary evaporation. The crude product was purified by flash chromatography (SiO2; DCM/MeOH; gradient 0-3%) to give the title compound.

WORKUP

后处理

  1. temperatureto cool
  2. filtrationthe mixture was filtered through a pad of Celite
  3. washThe filtrate was washed with water and brine
  4. dry with materialdried over MgSO4
  5. customthe solvent was removed by rotary evaporation
  6. customThe crude product was purified by flash chromatography (SiO2; DCM/MeOH; gradient 0-3%)