反应 #487494

反应方程式

dimethyl terephthalate

1-docosanol

→

product

收率 98.3%

didocosyl terephthalate

收率 98.3%

溶剂

methanol

反应条件

后处理

1. 1
   其他To a 3 neck 500 mL round bottomed flask equipped with a Dean Stark trap and condenser, thermocouple and argon inlet
2. 2
   温度The temperature was raised to 180° C
3. 3
   其他was collected
4. 4
   其他for ˜10 minutes
5. 5
   workup.DISTILLATIONwere distilled off
6. 6
   温度The solution was cooled under argon to about 140° C.
7. 7
   温度to cool to room temperature

实验过程

To a 3 neck 500 mL round bottomed flask equipped with a Dean Stark trap and condenser, thermocouple and argon inlet was added dimethyl terephthalate (49.57 grams, available from Sigma Aldrich), 1-docosanol (167.76 grams, available from Spectrum Chemical), Fascat 4100 (0.22 grams, available from Arkema Inc) and Xylenes (100 mL, available from Sigma Aldrich). The mixture was slowly heated under argon to 160° C. during which reagents melted. The temperature was raised to 180° C. The reaction mixture was stirred at 180° C. overnight (about 20 hours) during which 63 mL of a mixture of xylenes and methanol was collected. A vacuum was applied (1-2 mm-Hg) for ˜10 minutes during which all the Xylenes were distilled off. The solution was cooled under argon to about 140° C. and discharged in an aluminum tray where it was allowed to cool to room temperature to give 196.6 grams of product as an off-white solid (98% 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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