Reaktionsgleichung
[CH3:1][C:2]([N:7]1[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1)([CH3:6])[C:3]([NH2:5])=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[NH2:5][CH2:3][C:2]([N:7]1[CH2:12][CH2:11][O:10][CH2:9][CH2:8]1)([CH3:6])[CH3:1]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A solution of 8.33 g of 2-methyl-2-morpholino-propionic acid amide in 50 ml of tetrahydrofuran is slowly added at room temperature to 3.33 g of lithium aluminium hydride in 85 ml of tetrahydrofuran. The reaction mixture is then stirred for a further 2 hours under reflux. The reaction mixture is cooled and then 5 ml of water, 6.67 ml of 2N sodium hydroxide and a further 5 ml of water are added in succession. The suspension is clarified by filtration and the crude title compound is obtained from the concentrated filtrate: 1H NMR (CDCl3), δ(ppm)=3.67 (4H, m), 2.52 (2H, s), 2.48 (4H, m), 1.37 (2H, bs), 0.92 (6H, s).
Aufarbeitung
- temperatureunder reflux
- temperatureThe reaction mixture is cooled
- filtrationThe suspension is clarified by filtration
Quellen und Nachweise
- ORD-Eintrag
- ord-0d0cf0443de741748d0f67f204f74464
- Quelldatensatz
- uspto-grants-1998_01
- Patentnummer
- US05705658
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