Reaktion #220910

Reaktionsgleichung

phosphoric acid

water

Phosphoric Acid

triacetonamine

ethylene glycol

toluene

→

8,8,10,1 0-tetramethyl-1,5-dioxa-9-azaspiro[5.5]undecane

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was heated
2. 2
   Temperaturto reflux
3. 3
   Sonstigeformed
4. 4
   Sonstigewas removed on a water separator
5. 5
   SonstigeInstead, a plurality of secondary components had formed which

Vorschrift

Use of Phosphoric Acid 77 g of triacetonamine were initially charged in 240 g of toluene together with 47 g of ethylene glycol. Subsequently, sufficient phosphoric acid (63 g) was added that the reaction mixture showed an acidic pH (≦2) when tested with a moistened indicator paper. The reaction mixture was heated to reflux temperature and water of reaction formed was removed on a water separator. After approx. 3 hours, there was less than 10% of the desired product according to the gas chromatogram. Instead, a plurality of secondary components had formed which were not investigated further.

Quelle