반응 #10279

반응 방정식

aminoacetaldehyde dimethylacetal

5-chlorovaleryl chloride

sodium hydride

→

1-(2,2-dimethoxyethyl)-piperidin-2-one

수율 80.9%

용매

ethyl acetate

sodium carbonate

반응 조건

후처리

1. 1
   기타The aqueous layer was separated
2. 2
   추출extracted with ethyl acetate
3. 3
   세척The combined organic phase was washed with 1% hydrochloric acid and water
4. 4
   건조dried (magnesium sulfate)
5. 5
   농축concentrated
6. 6
   workup.DISSOLUTIONThe oily residue was dissolved in tetrahydrofuran
7. 7
   온도The reaction mixture was heated
8. 8
   온도under reflux for 1.5 hours
9. 9
   여과filtered
10. 10
    농축The filtrate was concentrated

실험 절차

To a stirred mixture of aminoacetaldehyde dimethylacetal (0.74 g, 7 mmole) in ethyl acetate (20 mL) and 2M sodium carbonate (20 mL) was added 5-chlorovaleryl chloride (1.55 g, 10 mmole). The reaction mixture was stirred at ambient temperature for 1 hour. The aqueous layer was separated and extracted with ethyl acetate. The combined organic phase was washed with 1% hydrochloric acid and water, dried (magnesium sulfate), and concentrated. The oily residue was dissolved in tetrahydrofuran, and sodium hydride (60% in oil) (0.3 g, 7.5 mmole) was added. The reaction mixture was heated under reflux for 1.5 hours and filtered. The filtrate was concentrated to give 1-(2,2-dimethoxyethyl)-piperidin-2-one (1.06 g) as a pale yellow oil.

출처