반응 #487493

반응 방정식

Dimethyl terephthalate

Stearyl Alcohol

→

white solid

수율 96.2%

distearyl terephthalate

수율 96.2%

반응 조건

후처리

1. 1
   기타To a 2 L Buchi reactor equipped with a double turbine agitator and distillation apparatus
2. 2
   기타purge for 1 hour
3. 3
   workup.ADDITIONwas commenced followed by the addition of Tyzor catalyst (3.0 grams, available from Dupont)
4. 4
   온도The reaction mixture was then heated to 145° C.
5. 5
   기타to 190° C.
6. 6
   기타over a 3-4 hour
7. 7
   workup.DISTILLATIONis distilled in a controlled manner
8. 8
   온도The reaction temperature was maintained at 190° C. for an additional 16 hours until >96% conversion to the product
9. 9
   온도on cooling

실험 절차

To a 2 L Buchi reactor equipped with a double turbine agitator and distillation apparatus was charged Dimethyl terephthalate (315.8 grams), Stearyl Alcohol (879.7 grams) and heated to 130° C. under Nitrogen purge for 1 hour, after which stirring was commenced followed by the addition of Tyzor catalyst (3.0 grams, available from Dupont). The reaction mixture was then heated to 145° C., followed by slowly ramping the temperature to 190° C. over a 3-4 hour period such that the evolution of methanol is distilled in a controlled manner. The reaction temperature was maintained at 190° C. for an additional 16 hours until >96% conversion to the product was achieved as determined by 1H NMR spectroscopy. The product was discharged as a low viscosity liquid which solidified on cooling to give a 1050 gram of a white solid (96.2% yield). The product was shown to be pure by 1H NMR spectroscopy with trace amounts of the mono-ester. Physical properties of this compound are shown in Table 2.

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