تفاعل #52056

معادلة التفاعل

2-Ethoxy-6-pentadecyl benzaldehyde

ethyl acetoacetate

Acetic acid

piperidine

Ethyl-3-amino crotonate

→

diethyl 1,4-dihydro-4-(2′-ethoxy-6′-pentadecyl phenyl)-2,6-dimethyl-3,5-pyridine dicarboxylate

المذيبات

n-butanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةrefluxed for 10 hrs
2. 2
   أخرىn-Butanol was evaporated
3. 3
   أخرىreaction mixture
4. 4
   غسيلwas washed with distilled water
5. 5
   استخلاصextracted with dichloromethane (10 mL)
6. 6
   تجفيفOrganic layer was dried over sodium sulfate
7. 7
   أخرىevaporated
8. 8
   أخرىcompound was purified by column chromatography

الإجراء التجريبي

2-Ethoxy-6-pentadecyl benzaldehyde (3 g, 8.3 mmol) and ethyl acetoacetate (1.08 g, 8.3 mmol) were dissolved in n-butanol (20 mL). Acetic acid (0.5 g, 8.3 mmol) and piperidine (0.7 g, 8.3 mmol) were added and stirred at room temperature for 3-4 hrs. Ethyl-3-amino crotonate (1.08 g, 8.3 mmol) was then added and refluxed for 10 hrs. n-Butanol was evaporated and reaction mixture was washed with distilled water and extracted with dichloromethane (10 mL). Organic layer was dried over sodium sulfate, evaporated and compound was purified by column chromatography using silicagel (100-200 mesh) with hexane:EtOAc (94:6) solvent system to give diethyl 1,4-dihydro-4-(2′-ethoxy-6′-pentadecyl phenyl)-2,6-dimethyl-3,5-pyridine dicarboxylate as white powder.

المصدر