反应 #52056

反应方程式

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

溶剂

n-butanol

反应条件

后处理

1. 1
   温度refluxed for 10 hrs
2. 2
   其他n-Butanol was evaporated
3. 3
   其他reaction mixture
4. 4
   洗涤was washed with distilled water
5. 5
   萃取extracted with dichloromethane (10 mL)
6. 6
   干燥Organic layer was dried over sodium sulfate
7. 7
   其他evaporated
8. 8
   其他compound was purified by column chromatography

实验过程

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.

来源