Reaktion #310685

Reaktionsgleichung

1,1-dimethylethylenediamine

phenylacetyl chloride

→

1,1-dimethyl-2-(2-phenylacetamido)ethylamine

Ausbeute 63.7%

Lösungsmittel

ether

ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solid was separated by filtration
2. 2
   workup.DISSOLUTIONdissolved in warm water (150 ml.)
3. 3
   SonstigeThe solution obtained
4. 4
   Filtrationwas filtered
5. 5
   workup.ADDITIONThe filtrate was basified by addition of an excess of saturated aqueous sodium carbonate solution (50 ml.)
6. 6
   Extraktionextracted with chloroform (3×250 ml.)
7. 7
   TrocknenThe extracts were dried (MgSO4)
8. 8
   Sonstigeevaporated
9. 9
   Sonstigeto give an oil which
10. 10
    Sonstigecrystallised on addition of a 1:1 v/v mixture of ether and petrol (60°-80°)

Vorschrift

A solution of 1,1-dimethylethylenediamine (8.8 g.) in ether (250 ml.) was added during 2 hours to a stirred solution of phenylacetyl chloride (15.4 g.) in ether (250 ml.). This mixture was further stirred for 2 hours. The solid was separated by filtration, and dissolved in warm water (150 ml.). The solution obtained was filtered. The filtrate was basified by addition of an excess of saturated aqueous sodium carbonate solution (50 ml.), and then extracted with chloroform (3×250 ml.). The extracts were dried (MgSO4) and evaporated to give an oil which crystallised on addition of a 1:1 v/v mixture of ether and petrol (60°-80°) to give 1,1-dimethyl-2-(2-phenylacetamido)ethylamine (13.1 g., 63%), m.p. 47°-48° C.

Quelle