반응 #652859

반응 방정식

water

2-bromomethyl-2,3-dihydro-2,4,6,7-tetramethyl-5-benzofuranamine

3-(1,2,3,6-tetrahydro-4-pyridyl)-1H-indole

potassium bicarbonate

→

title compound

수율 82.4%

2,3-Dihydro-2,4,6,7-tetramethyl-2-[[1,2,3,6-tetrahydro-4-(3-indolyl)-1-pyridyl]methyl]-5-benzofuranamine

수율 82.4%

용매

N,N-dimethylactamide

반응 조건

후처리

1. 1
   온도was refluxed for 7.5 hours under nitrogen atmosphere
2. 2
   추출the product was extracted twice with ethyl acetate
3. 3
   추출The combined extract
4. 4
   세척was washed with water
5. 5
   건조dried over anhydrous magnesium sulfate
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   기타The residue was purified by basic silica gel column chromatography (hexane:ethyl acetate=1:1)
9. 9
   기타recrystallized from acetone/diisopropyl ether

실험 절차

A suspension of 2-bromomethyl-2,3-dihydro-2,4,6,7-tetramethyl-5-benzofuranamine (0.85 g), 3-(1,2,3,6-tetrahydro-4-pyridyl)-1H-indole (1.1 g) and potassium bicarbonate (0.83 g) in N,N-dimethylactamide (6 mL) was refluxed for 7.5 hours under nitrogen atmosphere. To the mixture water was added and the product was extracted twice with ethyl acetate. The combined extract was washed with water followed by saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, filtered and evaporated. The residue was purified by basic silica gel column chromatography (hexane:ethyl acetate=1:1) and recrystallized from acetone/diisopropyl ether to provide 0.99 g of the title compound. Yield 82%.

출처