A kind of chemical resolution preparation method of S-configuration pregabalin
A technology for pregabalin and chemical separation, applied in chemical instruments and methods, cyanide reaction preparation, organic compound preparation, etc., to achieve the effects of easy recycling, high resolution efficiency, and simple operation
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Embodiment 1
[0039] In a 50mL three-neck flask, 1.29g of L-pyroglutamic acid and 1.59g of pregabalin racemate were dissolved in 24mL of ethanol solution with a volume ratio of 50%, heated to 50-60°C to dissolve, kept warm and stirred for 0.5h, and cooled naturally for 30- 35 ℃, crystallization 4h. Suction filtration, transfer the obtained solid into 5mL ethanol solution with a volume ratio of 50%, keep stirring at 50°C for 1h, cool to 30°C, crystallize for 1h, suction filtration, and dry to obtain 1.32g of S-pregabalin and L-pregabalin Pyroglutamate complex.
[0040] Suspend 1.32g of the above-mentioned salt complex in 13mL of deionized water, heat to 40-50°C, then add 10% hydrochloric acid and adjust the pH=0.5-1, stir at room temperature for 0.5h, extract with ethyl acetate, and recover the resolving agent L - Pyroglutamate. The pH of the aqueous layer was adjusted to neutral with 20% sodium hydroxide. Concentrate about 8mL of water under reduced pressure. At this time, a small amount...
Embodiment 2
[0042] In a 5L three-necked flask, 129g of L-pyroglutamic acid and 159g of pregabalin racemate were dissolved in 2L of ethanol solution with a volume ratio of 50%, heated to 50-60°C to dissolve, kept warm and stirred for 1 hour, and cooled naturally to 30-35°C. Crystallization 4h. After suction filtration, the filter cake was washed with 50% by volume ethanol solution and dried to obtain 129 g of S-pregabalin and L-pyroglutamate complex.
[0043] Suspend 129g of the above salt complex in 1.1L deionized water, heat to 40-50°C, then add 10% hydrochloric acid and adjust the pH=0.5-1, stir at room temperature for 0.5h, extract with ethyl acetate, and recover the resolving agent L - Pyroglutamate. The pH of the aqueous layer was adjusted to neutral with 20% sodium hydroxide. Concentrate about 800mL of water under reduced pressure. At this time, a small amount of crystals precipitated, stop the concentration, lower the temperature to 0-5°C, keep warm and crystallize for 4h, filter, ...
Embodiment 3
[0045] In a 50mL three-necked flask, 1.29g of L-pyroglutamic acid and 1.59g of pregabalin racemate were dissolved in 20mL of ethanol solution with a volume ratio of 60%, heated to 40-50°C to dissolve, kept warm and stirred for 0.5h, and cooled to room temperature naturally , Crystallization 4h. After suction filtration, the filter cake was washed with 60% by volume ethanol solution and dried to obtain 1.03 g of S-pregabalin and L-pyroglutamate complex.
[0046] Suspend 1.03 g of the above salt complex in 10 mL of deionized water, heat to 40-50 °C, then add 10% hydrochloric acid and adjust the pH to 0.5-1, stir at room temperature for 0.5 h, extract with dichloromethane, and recover the resolving agent L - Pyroglutamate. The pH of the aqueous layer was adjusted to neutral with 10% sodium hydroxide. Concentrate about 9 mL of water under reduced pressure. At this time, a small amount of crystals precipitated, stop the concentration, lower the temperature to 0-5°C, keep warm and...
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