1-Acetyl-3-azetidinecarboxylic acid synthesis
- Product Name:1-Acetyl-3-azetidinecarboxylic acid
- CAS Number:97628-91-6
- Molecular formula:C6H9NO3
- Molecular Weight:143.14
97628-91-6
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$20.00/250mg
36476-78-5
418 suppliers
$6.00/1g
Yield:36476-78-5 27.9%
Reaction Conditions:
with palladium 10% on activated carbon;hydrogen in ethanol at 40; under 15001.5 Torr; for 24 h;
Steps:
16
General procedure: At room temperature, in a three-necked flask, 95.3 g of 1-benzylazetidin-3-carbaldehyde in step (1), a tetrahydrofuran solution, and purified water were sequentially added, and mechanical stirring was started.Reduce the temperature to 0 ° C and slowly add 37.7 g of sodium chlorite.The temperature was raised to 20-30 ° C for 15-20 hours. After the reaction was completed, ethyl acetate was added for extraction.After extraction and concentration under reduced pressure, the intermediate 1-benzylazetidine-3-carboxylic acid was obtained.Add 1-benzylazetidin-3-carboxylic acid, ethanol,10% palladium carbon, heated to 40 ° C, hydrogen gas was passed in, and the pressure was controlled at 2 MPa for 24 hours.After the reaction, the palladium carbon was filtered, and the ethanol was concentrated under reduced pressure to obtain a crude azetidine-3-carboxylic acid.Recrystallized from ethyl acetate, filtered, the filter cake was rinsed with ethyl acetate, dried,35.3 g of pure azetidine-3-carboxylic acid was obtained,The yield was 82.8%, and the GC purity was 99.2%.
References:
CN110437118,2019,A Location in patent:Paragraph 0084-0087; 0102-0103