تفاعل #569257

معادلة التفاعل

1-octadecanol

ethyl 4-aminobenzoate

p-toluenesulfonic acid

→

off-white waxy material

المردود 121.9%

Octadecyl-4-Aminobenzoate

المردود 121.9%

المذيبات

ظروف التفاعل

المعالجة

1. 1
   أخرىA 1-liter round bottom flask was fitted with a reflux condenser
2. 2
   درجة الحرارةDean Stark trap and heating mantle
3. 3
   أخرىThe flask was flushed with nitrogen
4. 4
   أخرىsealed under a nitrogen balloon
5. 5
   درجة الحرارةThe reaction system was heated
6. 6
   درجة الحرارةto reflux for about 1/2 hour before a 25 ml-aliquot of xylenes-ethanol mixture
7. 7
   أخرىwas removed through the Dean-Stark trap
8. 8
   أخرىEvery 5-10 minutes, another 25 ml aliquot of the xylenes-ethanol mixture was removed until a total of 400 ml
9. 9
   أخرىhad been withdrawn from the reaction mixture
10. 10
    أخرىa temperature of 150° C
11. 11
    أخرىRemaining volatiles were removed under 29 inches of Hg vacuum at 70° C. in a vacuum oven

الإجراء التجريبي

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 Every 5-10 minutes, another 25 ml aliquot of the xylenes-ethanol mixture was removed until a total of 400 ml had been withdrawn from the reaction mixture and the pot attained a temperature of 150° C. Remaining volatiles were removed under 29 inches of Hg vacuum at 70° C. in a vacuum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

المصدر