反応 #471034

反応方程式

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

溶媒

Ethyl acetate

toluene

反応条件

後処理

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

実験手順

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.

出典