반응 #90467

반응 방정식

KOH

1,3-dibromopropane

3,6-dibromocarbazole

→

colorless oil

수율 28.6%

3,6-dibromo-9-(3-bromopropyl)-9H-carbazole

수율 28.6%

용매

EtOAc

DMF

DMF

반응 조건

후처리

1. 1
   workup.STIRRINGwas stirred at room temperature overnight
2. 2
   기타The crude reaction mixture
3. 3
   세척washed with 1M HCl2×10 mL and water 3×10 mL
4. 4
   건조The organic layer was dried over anhydrous Na2SO4
5. 5
   기타evaporated
6. 6
   기타to afford the crude product, which

실험 절차

Crushed KOH (0.0673 g, 1.20 mmol, 1.2 equiv) was added to 3,6-dibromocarbazole (0.3250 g, 1.00 mmol) in 2 mL DMF solution and the mixture was stirred for 30 min. 1,3-dibromopropane (0.5047 g, 2.50 mmol, 2.5 equiv) in 3 mL DMF solution was added dropwise into the mixture and it was stirred at room temperature overnight. The crude reaction mixture was diluted with 30 mL EtOAc and washed with 1M HCl2×10 mL and water 3×10 mL. The organic layer was dried over anhydrous Na2SO4 and evaporated to afford the crude product, which was subjected to silica gel chromatography using Hexanes/EtOAc to afford 0.1275 g colorless oil as product, yield 28.6%.

출처