反应 #471034

反应方程式

7-Bromo-5-methoxy-N,N-dimethylbenzofuran-2-carboxamide

1-(2-pyridin-2-yl-ethyl)piperazine

2-dicyclohexylphosphino-2′,4′,6′-tri-iso-propyl-1,1′-biphenyl

sodium t-butoxide

→

title compound

5-Methoxy-N,N-dimethyl-7-(4-(2-(pyridin-2-yl)ethyl)piperazin-1-yl)benzofuran-2-carboxamide

溶剂

Ethyl acetate

toluene

反应条件

后处理

1. 1
   温度to cool
2. 2
   过滤the mixture was filtered through a pad of Celite
3. 3
   洗涤The filtrate was washed with water and brine
4. 4
   干燥dried over MgSO4
5. 5
   其他the solvent was removed by rotary evaporation
6. 6
   其他The crude product was purified by flash chromatography (SiO2; DCM/MeOH; gradient 0-3%)

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.

来源