Reaktion #11289

Reaktionsgleichung

3-methyl-cyclohex-1-ene-4-methanol

decalin

methyl acrylate

→

ethylene/methyl acrylate methyl cyclohexene methyl acrylate

Lösungsmittel

CHCl3

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONTo this was added 350 g of Chevron EMAC SP-2260 which
2. 2
   TemperaturThe temperature of the mixture was gradually raised
3. 3
   Sonstigereached approximately 120° C.
4. 4
   Sonstigereached approximately 140° C.
5. 5
   workup.STIRRINGwhile stirring
6. 6
   SonstigeAfter 5 hours of reaction
7. 7
   Temperaturthe mixture was cooled
8. 8
   Sonstigethe mixture was then precipitated
9. 9
   workup.ADDITIONby adding it to 4 liters of CH3OH in a Waring blender
10. 10
    FiltrationThe precipitate is filtered
11. 11
    Waschenwashed with CH3OH
12. 12
    Sonstigedried in a vacuum oven at 50° C

Vorschrift

550 ml of decalin® was placed in a flask. To this was added 350 g of Chevron EMAC SP-2260 which has 24 weight % of methyl acrylate (0.9767 moles of methyl acrylate) and 0.48 g of Irganox®1076 (0.1 mole). The temperature of the mixture was gradually raised while stirring. When the temperature reached approximately 120° C., 127.1 g (0.9767 moles) of 3-methyl-cyclohex-1-ene-4-methanol (97%) was added. When the temperature reached approximately 140° C., 4.8 g of the catalyst Ti(OC2H5)4 was added a portion at a time. The temperature was maintained at 170° C. while stirring. The course of the reaction was observed by subjecting samples of the mixture to NMR at hourly intervals. The percent conversion is given in Table 1 below. After 5 hours of reaction, the mixture was cooled and 400 ml of CHCl3 was added and the mixture was then precipitated by adding it to 4 liters of CH3OH in a Waring blender. The precipitate is filtered and washed with CH3OH and dried in a vacuum oven at 50° C. The dried mixture yielded 407.5 g of ethylene/methyl acrylate/methyl cyclohexene methyl acrylate (EMCM).

Quelle