N-Carbethoxy-4-piperidone synthesis
- Product Name:N-Carbethoxy-4-piperidone
- CAS Number:29976-53-2
- Molecular formula:C8H13NO3
- Molecular Weight:171.19
53601-94-8
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Yield:29976-53-2 98.2%
Reaction Conditions:
with hydrogenchloride in ethanol;water at 83 - 85; for 7 h;
Steps:
1.4
The specific operations of step four include: 1 mmol of compound 3,10 mL of ethanol,3 mL of 20% hydrochloric acid was added to a 100 mL three-necked flask equipped with a reflux condenser and a thermometer.heating,83-85 reflux,After 1 h, the color of the solution changed from colorless to pale yellow and gradually deepened.The progress of the reaction was monitored by thin layer chromatography.After 6 h, the reaction was complete.After the reaction liquid is cooled,Extract three times with dichloromethane,Combine the organic phase,Washed to neutral,Dry with anhydrous sodium sulfate,filter,The filtrate was spun dry using a rotary evaporator.The obtained crude product was separated by silica gel column chromatography.Obtaining a colorless liquid, Compound 4,The yield was 98.2%.
References:
CN108191741,2018,A Location in patent:Paragraph 0028
