تفاعل #2828

معادلة التفاعل

pyridine

methyl 3-aminobenzoate

valeryl chloride

→

methyl 3-valeramidobenzoate

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwhile cooling on ice
2. 2
   استخلاصThe whole was extracted with ethyl acetate
3. 3
   غسيلwashed with 5% sodium hydrogencarbonate aqueous solution and water
4. 4
   تجفيفdried over anhydrous sodium sulfate
5. 5
   أخرىThe solvent was evaporated
6. 6
   أخرىthe residue was purified by silica gel column chromatography (Kieselgel 60=170 g, hexane/ethyl acetate=3/1)
7. 7
   أخرىto obtain the above-captioned compound ([6]-(62)-90) (7.70 g) as a white solid

الإجراء التجريبي

To anhydrous pyridine (120 ml), methyl 3-aminobenzoate (5.00 g) was dissolved, and valeryl chloride (4.13 ml) was added while cooling on ice. The mixture was stirred at room temperature for 4 hours. Distilled water was added to the solution. The whole was extracted with ethyl acetate, washed with 5% sodium hydrogencarbonate aqueous solution and water, and dried over anhydrous sodium sulfate. The solvent was evaporated, and the residue was purified by silica gel column chromatography (Kieselgel 60=170 g, hexane/ethyl acetate=3/1) to obtain the above-captioned compound ([6]-(62)-90) (7.70 g) as a white solid.

المصدر