Reaktion #667782

Reaktionsgleichung

1,1'-ethylenebis(3,3,5,5-tetramethyl-2-piperazinone)

N,N'-(2-amino-2-methylpropyl)ethylenediamine

acetone cyanohydrin

acetic anhydride

→

above-named product

1,1'-Ethylenebis(4-acetyl-3,3,5,5-tetramethyl-2-piperazinone)

Lösungsmittel

Methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled to room temperature
2. 2
   Extraktionto extract the product into an organic layer which
3. 3
   Waschenis then washed successively with water and with saturated sodium bicarbonate solution
4. 4
   Trocknenis finally dried over anhydrous magnesium sulfate
5. 5
   SonstigeThe solvent is removed in vacuo
6. 6
   Sonstigethe residual product is recrystallized from toluene

Vorschrift

31.5 grams (0.1 mole) of 1,1'-ethylenebis(3,3,5,5-tetramethyl-2-piperazinone), prepared according to Example 6, E of U.S. Pat. No. 4,190,571 from N,N'-(2-amino-2-methylpropyl)ethylenediamine and acetone cyanohydrin, is dissolved in 102 grams (1.0 mole) of acetic anhydride. After three drops of concentrated sulfuric acid are added to the solution, the mixture is heated for four hours at 130° C. and then cooled to room temperature. Methylene chloride (200 ml.) is added to extract the product into an organic layer which is then washed successively with water and with saturated sodium bicarbonate solution and is finally dried over anhydrous magnesium sulfate. The solvent is removed in vacuo and the residual product is recrystallized from toluene to give 30.4 grams of the above-named product as a white solid, melting at 180°-183° C. (sintering at 170° C.).

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