Method for synthesizing (S)-2-aminobutanamide
A technology of aminobutyramide and synthesis method, which is applied in the direction of organic chemical method, carboxylic acid amide preparation, chemical instrument and method, etc., can solve the problems of difficult separation of by-products, control of environmental pollution, difficult operating conditions, etc., and achieve atom utilization High efficiency, short process route and convenient operation
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Embodiment 1
[0021] Add 103.1g (1.0mol) of 2-aminobutyric acid and 76.1g (0.5mol) of D-mandelic acid in a dried 500ml four-necked flask equipped with a mechanical stirring device and a thermometer, and then add 300.0g of methanol. Turn on the stirring, raise the temperature to 60° C., and finish the reaction in 3 hours. After the reaction was completed, the temperature of the reaction liquid was lowered to 0° C., and filtered to obtain (S)-2-aminobutyric acid D-mandelate.
[0022] Add the obtained (S)-2-aminobutyric acid D-mandelate into the reaction flask, then add 200g of methyl tert-butyl ether and 100g of water, stir, and adjust the pH of the solution to 4~5. After the adjustment is completed, Liquid separation. Collect the water layer, concentrate under reduced pressure and distill 80 g of water, add 5 g of sodium chloride, and keep stirring at 20° C. for 2 hours. After filtering, the filter cake was dried in a vacuum oven at 40°C. 37.0 (S)-2-aminobutyric acid was obtained in a yie...
Embodiment 2
[0026] Add 103.1g (1.0mol) of 2-aminobutyric acid and 197.5g (0.6mol) of D-camphorsulfonic acid in a dried 1000ml four-necked flask equipped with a mechanical stirring device and a thermometer, and then add 500.0g of ethanol. Turn on the stirring, raise the temperature to 65° C., and finish the reaction in 3 hours. After the reaction was completed, the temperature of the reaction liquid was lowered to 0° C., and filtered to obtain (S)-2-aminobutyric acid dextrocamphorsulfonate.
[0027] Add the obtained (S)-2-aminobutyric acid dextrocamphorsulfonate to the reaction flask, then add 500g of ethyl acetate and 200g of water, stir, and adjust the pH of the solution to 4~5. After the adjustment is completed, separate the liquids . Collect the water layer, concentrate under reduced pressure and distill 160 g of water, add 5 g of sodium chloride, and keep stirring at 20° C. for 2 hours. After filtering, the filter cake was dried in a vacuum oven at 40°C. 36.1 (S)-2-aminobutyric aci...
Embodiment 3
[0031] Add 103.1g (1.0mol) of 2-aminobutyric acid and 197.5g (0.6mol) of D-camphorsulfonic acid in a dried 1000ml four-neck flask equipped with a mechanical stirring device and a thermometer, and then add 500.0g of isopropanol . Turn on the stirring, raise the temperature to 65° C., and finish the reaction in 3 hours. After the reaction was completed, the temperature of the reaction liquid was lowered to 0° C., and filtered to obtain (S)-2-aminobutyric acid dextrocamphorsulfonate.
[0032] Add the obtained (S)-2-aminobutyric acid dextrocamphorsulfonate to the reaction flask, then add 500g of ethyl acetate and 200g of water, stir, and adjust the pH of the solution to 4~5. After the adjustment is completed, separate the liquids . Collect the water layer, concentrate under reduced pressure and distill 160 g of water, add 5 g of sodium chloride, and keep stirring at 20° C. for 2 hours. After filtering, the filter cake was dried in a vacuum oven at 40°C. 32.1 (S)-2-aminobutyric...
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