Decalin → Ethylene/methyl acrylate methyl cyclohexene methyl acrylate

関与物質

反応条件

反応手順

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).

情報源と証拠