Reaktion #574647

Reaktionsgleichung

4-aminobutyraldehyde-diethylacetal

sodium hydrogen carbonate

acetyl chloride

→

4-(N-acetylamino)butyraldehyde-diethylacetal

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organic phase is separated off
2. 2
   Extraktionthe aqueous phase is extracted twice more with dichloromethane
3. 3
   Trocknendried over MgSO4
4. 4
   Filtrationfiltered
5. 5
   Einengenconcentrated by evaporation in a rotary evaporator
6. 6
   SonstigeThe residue is purified by chromatography on silica gel with ethyl acetate

Vorschrift

35.8 g (0.2 mol) of 4-aminobutyraldehyde-diethylacetal (90%) are dissolved in 600 ml of dichloromethane, 300 ml of saturated sodium hydrogen carbonate solution are added, and the mixture is cooled to 0° C. 17 ml (0.24 mol) of acetyl chloride are added dropwise at 0°-5° C., and the mixture is stirred for a further 6 hours at 0°-5° C. The organic phase is separated off and the aqueous phase is extracted twice more with dichloromethane. The organic phases are combined, dried over MgSO4, filtered and concentrated by evaporation in a rotary evaporator. The residue is purified by chromatography on silica gel with ethyl acetate. 4-(N-acetylamino)butyraldehyde-diethylacetal is obtained in the form of a yellowish oil.

Quelle