Lithium Hydroxide → N-(2-fluoroethyl)-N-methyloxamic acid
Reaktionsgleichung
[F:1][CH2:2][CH2:3][N:4]([CH3:12])[C:5](=[O:11])[C:6]([O:8]CC)=[O:7].[Li+].[OH-]>CO.O>[F:1][CH2:2][CH2:3][N:4]([CH3:12])[C:5](=[O:11])[C:6]([OH:8])=[O:7]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a solution of ethyl 2-((2-fluoroethyl)(methyl)amino)-2-oxoacetate (1.2 g, 7.36 mmol) in methanol/water (30 mL, 1:1) was added LiOH (0.352 g, 14.71 mmol). The solution was stirred for 2 h. The methanol was removed by concentration and concentrated HCl (2 mL) was added. The solvent was removed and the residue dissolved in CH2Cl2 and filtered. The filtrate was concentrated to give the title compound as an off-white crystalline powder (0.615 g, 56% yield). 1H NMR (400 MHz, CDCl3) δ: 4.47-4.89 (2 H, m) 3.67-4.39 (2 H, m) 3.07-3.60 (3 H, m).
Aufarbeitung
- customThe methanol was removed by concentration and concentrated HCl (2 mL)
- additionwas added
- customThe solvent was removed
- dissolutionthe residue dissolved in CH2Cl2
- filtrationfiltered
- concentrationThe filtrate was concentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-e959f6e3c945458ea2af07eda1ca0a8e
- Quelldatensatz
- uspto-grants-2012_03
- Patentnummer
- US08129398B2
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