反应详情

温度

140 °C

A 1-liter round bottom flask was fitted with a reflux condenser, Dean Stark trap and heating mantle and charged with 54 g (0.20 mole) of 1-octadecanol, 33 g (0.20 mole) ethyl 4-aminobenzoate, 8 g of p-toluenesulfonic acid and 500 ml of mixed xylenes. The flask was flushed with nitrogen and sealed under a nitrogen balloon. The reaction system was heated to reflux with a pot temperature of about 140° C. and allowed to reflux for about 1/2 hour before a 25 ml-aliquot of xylenes-ethanol mixture was removed through the Dean-Stark trap. Every 5-10 minutes, another 25 ml aliquot of the xylenes-ethanol mixture was removed until a total of 400 ml had been withdrawn from the reaction mixture and the pot attained a temperature of 150° C. Remaining volatiles were removed under 29 inches of Hg vacuum at 70° C. in a vacuum oven to give 95 g of an off-white waxy material melting at 60°-70° C., with an infrared spectrum showing the amino-aromatic ester with a long-chain aliphatic tail.

1. customA 1-liter round bottom flask was fitted with a reflux condenser
2. temperatureDean Stark trap and heating mantle
3. customThe flask was flushed with nitrogen
4. customsealed under a nitrogen balloon
5. temperatureThe reaction system was heated
6. temperatureto reflux for about 1/2 hour before a 25 ml-aliquot of xylenes-ethanol mixture
7. customwas removed through the Dean-Stark trap
8. customEvery 5-10 minutes, another 25 ml aliquot of the xylenes-ethanol mixture was removed until a total of 400 ml
9. customhad been withdrawn from the reaction mixture
10. customa temperature of 150° C
11. customRemaining volatiles were removed under 29 inches of Hg vacuum at 70° C. in a vacuum oven