Chiral intermediate (S, S)-3-amino-N-cyclopropyl-2-hydroxyalkanamide or its salt and preparation method thereof
A technology of hydroxycaproylamide and cyclopropyl, applied in the field of preparation of chiral intermediate (S,S)-3-amino-N-cyclopropyl-2-hydroxycaproylamide or its salt, can solve the problem Stability, difficult crystallization and other problems, to achieve high yield, low cost, and reduce energy consumption
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Embodiment 1
[0028] Add 1.5 g of water and 30 g of the compound of formula II into a 250 ml three-necked reaction flask, then add 23 g of D-tartaric acid and 90 ml of ethanol, add 40 ml of acetic acid under stirring, heat up and reflux for about 2 hours, then cool down to 25-30°C and stir for crystallization. After filtering, the filter cake was soaked in ethanol, then filtered, and dried to constant weight to obtain 22.3 g of the crude compound of formula III as a white solid, EE: 87.2%, yield: 41%.
[0029]
Embodiment 2
[0031] Add 22.3g of the crude compound of formula III obtained in the example into a mixed solution of 100ml of ethanol and 12ml of water, stir and raise the temperature to 60-65°C, then keep it warm for 45 minutes, then cool down to 20-25°C, crystallize, filter, and the mother liquor Save it for later use, wash the filter cake, and dry to obtain 17.5 g of the fine compound of formula III, EE: 99.8%, and the yield is 79%.
[0032] The product in the above mother liquor was recovered to obtain 2 g of the refined compound of formula III, EE: 99.9%.
Embodiment 3
[0034] Add 30g of the compound represented by formula III to a 1L four-necked reaction flask, then add 490g of chloroform, control the temperature at 20-25°C and stir for 45 minutes, filter to remove the solid, and concentrate the mother liquor to dryness at 40°C under a pressure of -0.09MaP , to obtain the crude product of the compound shown in formula I.
[0035] The crude compound represented by formula I was added to 150 g of absolute ethanol, heated to 50-55° C. and stirred for 1 hour, then cooled to 20-25° C. for crystallization, and filtered to obtain the refined compound represented by formula I.
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