반응 #10275

반응 방정식

sodium hydride

azocan-2-one

5-bromo-1-pentene

→

1-pent-4-enyl-azocan-2-one

수율 94.4%

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.STIRRINGThe reaction mixture was stirred at room temperature for 30 minutes
2. 2
   workup.WAITat 80° C. for 16 hours
3. 3
   기타The solvent was removed under reduced pressure and water
4. 4
   workup.ADDITIONwas added to the residue
5. 5
   추출The mixture was extracted with ethyl ether
6. 6
   세척the organic phase was washed with water
7. 7
   건조dried (magnesium sulfate)
8. 8
   농축concentrated

실험 절차

To a stirred suspension of sodium hydride (0.9 g, 37.5 mmole) in dimethylformamide (50 mL) was added azocan-2-one (3.83 g, 30 mmole). The mixture was stirred at room temperature for 15 minutes, and then 5-bromo-1-pentene (5.03 g, 33.7 mmole) was added slowly. The reaction mixture was stirred at room temperature for 30 minutes, and then at 80° C. for 16 hours. The solvent was removed under reduced pressure and water was added to the residue. The mixture was extracted with ethyl ether, the organic phase was washed with water, dried (magnesium sulfate) and concentrated to give 1-pent-4-enyl-azocan-2-one (5.53 g,) as an oil.

출처