(S)-2-methylaminobutanoic acid synthesis
- Product Name:(S)-2-methylaminobutanoic acid
- CAS Number:88930-11-4
- Molecular formula:C5H11NO2
- Molecular Weight:117.15
146087-16-3
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Yield:88930-11-4 85.14 %
Reaction Conditions:
with piperidine in N,N-dimethyl-formamide at 5 - 25;
Steps:
73 Example 73, Preparation and Purification of (S)-2-(Methylamino)butanoic Acid
Reaction steps: Add 80mL of N,N-dimethylformamide and 58.85g of the compound of formula c-1 into a 500mL reactor at room temperature, and start stirring.Cool down to an internal temperature of 5-10°C, add 10 mL of piperidine dropwise, and keep stirring for 30 minutes after the drop is complete.Raise the temperature to an internal temperature of 20-25°C, keep stirring for 2-5h.Post-treatment steps: Add 160mL ethylene oxide to the system and stir for 10min. Cool down to internal temperature -10-5°C, keep stirring for 2 hours. Filtrate to obtain a white wet solid, and dry it under vacuum at 45°C for 24 hours to obtain a crude product.Purification steps: Add the crude product to a 500mL reactor at room temperature, add water to dissolve, then add cyclohexanone, keep stirring for 1 hour, and centrifuge.Add 20mL cyclohexanone to the reaction kettle, rinse the kettle wall, keep stirring for 30min,Wash the filter cake with the lotion, centrifuge to obtain a white wet solid, and dry the material under vacuum at 45°C for 24 hours.The finished product was 23.27g, the yield was 85.14%, and the purity was 96.78%.
References:
CN115466189,2022,A Location in patent:Paragraph 0060-0063
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