Diethyl Ether → N-(4-propyl-1,3-dioxolan-2-ylmethyl)-2-methoxy-alpha-chloroacetanilide
Reaktionsgleichung
[CH2:1]([CH:4]1[CH2:8][O:7][CH:6]([CH2:9][NH:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2OC)[O:5]1)[CH2:2][CH3:3].[CH2:19]([O:21][CH2:22]C)C.[C:24](=[O:27])([O-])[O-].[Na+].[Na+].[Cl:30]CC(Cl)=O>O>[CH2:1]([CH:4]1[CH2:8][O:7][CH:6]([CH2:9][N:10]([C:24](=[O:27])[CH:19]([O:21][CH3:22])[Cl:30])[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[O:5]1)[CH2:2][CH3:3]Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 5 °C
Versuchsvorschrift
N-(4-Propyl-1,3-dioxolan-2-ylmethyl)-2-methoxyaniline (0.25 mole), diethyl ether (30 ml), sodium carbonate (35.5 grams) and water (50 ml) are charged into a glass reaction vessel equipped with stirrer, thermometer and cooling means. The mixture is cooled to about 5° C. and chloroacetyl chloride (0.28 mole) is added dropwise with stirring. After the addition is completed, stirring is continued for 1 hour. After this time the organic phase is separated from the aqueous phase and is filtered. The filtrate is then washed with aqueous sodium carbonate, dried over anhydrous magnesium sulfate and filtered. The filtrate is then stripped of solvent under reduced pressure to yield the desired product N-(4-propyl-1,3-dioxolan-2-ylmethyl)-2-methoxy-α-chloroacetanilide as the residue.
Aufarbeitung
- customequipped with stirrer
- temperaturethermometer and cooling means
- additionAfter the addition
- stirringstirring
- customAfter this time the organic phase is separated from the aqueous phase
- filtrationis filtered
- washThe filtrate is then washed with aqueous sodium carbonate
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
Quellen und Nachweise
- ORD-Eintrag
- ord-014ae2fa5ffd4701817a05d6204d0400
- Quelldatensatz
- uspto-grants-1980_09
- Patentnummer
- US04225335
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