반응 #569257

반응 방정식

1-octadecanol

ethyl 4-aminobenzoate

p-toluenesulfonic acid

→

off-white waxy material

수율 121.9%

Octadecyl-4-Aminobenzoate

수율 121.9%

용매

반응 조건

후처리

1. 1
   기타A 1-liter round bottom flask was fitted with a reflux condenser
2. 2
   온도Dean Stark trap and heating mantle
3. 3
   기타The flask was flushed with nitrogen
4. 4
   기타sealed under a nitrogen balloon
5. 5
   온도The reaction system was heated
6. 6
   온도to reflux for about 1/2 hour before a 25 ml-aliquot of xylenes-ethanol mixture
7. 7
   기타was removed through the Dean-Stark trap
8. 8
   기타Every 5-10 minutes, another 25 ml aliquot of the xylenes-ethanol mixture was removed until a total of 400 ml
9. 9
   기타had been withdrawn from the reaction mixture
10. 10
    기타a temperature of 150° C
11. 11
    기타Remaining volatiles were removed under 29 inches of Hg vacuum at 70° C. in a vacuum oven

실험 절차

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 Every 5-10 minutes, another 25 ml aliquot of the xylenes-ethanol mixture was removed until a total of 400 ml had been withdrawn from the reaction mixture and the pot attained a temperature of 150° C. Remaining volatiles were removed under 29 inches of Hg vacuum at 70° C. in a vacuum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.

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