Reaktion #347022

Reaktionsgleichung

trimethylhydroquinone

CO2

isophytol

→

α-tocopherol

Ausbeute 84.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigecondensed in
2. 2
   Sonstigeresulted in a pressure of 185 bar
3. 3
   Sonstigewere injected by means of an HPLC pump over the course of 1.5 hours (h) at 108° C
4. 4
   Temperaturthe autoclave was cooled to room temperature (RT)
5. 5
   SonstigeThe ion exchanger was removed from the product by centrifuging the mixture

Vorschrift

15.02 g (98.8 mmol) of trimethylhydroquinone and 10.59 g of the strongly acid ion exchanger Amberlyst A15 were placed in a 300 ml autoclave, and 116 g of CO2 were condensed in. Heating to 100° C. resulted in a pressure of 185 bar. 37.80 ml (29.48 g; 99.6 mmol) of isophytol were injected by means of an HPLC pump over the course of 1.5 hours (h) at 108° C. After stirring at 108° C. for a further 30 minutes (min), the autoclave was cooled to room temperature (RT), and the pressure was released. The ion exchanger was removed from the product by centrifuging the mixture. The 48.9 g of isolated pale yellow oil contained 83% tocopherol, which corresponds to an 84% yield of pure α-tocopherol.

Quelle