Novel crystal form D of Retigabine and preparation method thereof
A technology of retigabine and crystal form, applied in the field of medicinal chemistry, can solve the problems of uncertain bioavailability, non-specific crystal form, difficult quality control, etc., to avoid pollution and change of drug properties, reduce production costs, The effect of reducing production links
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Embodiment 1
[0028] Add 2kg retigabine and 8L diethyl ether into the dissolving tank, stir at room temperature until the solids are completely dissolved, filter, pump the filtrate into the crystallization tank, cool to -10°C to 0°C, stir and crystallize for 4 hours, and filter with a centrifuge. Washed with ether for 3 times, spin-dried, and dried under reduced pressure to obtain 1.83 kg of new crystal form D of retigabine.
Embodiment 2
[0030] Add 2kg retigabine and 8L diethyl ether into the dissolution tank, stir at room temperature until the solids are completely dissolved, filter, pump the filtrate into the crystallization tank, cool to 0°C to 10°C, stir and crystallize for 4 hours, filter with a centrifuge, diethyl ether Washed 3 times, dried, and dried under reduced pressure to obtain 1.85 kg of retigabine new crystal form D.
Embodiment 3
[0032] Add 2kg retigabine and 12L isopropyl ether into the dissolution tank, stir at room temperature until the solids are completely dissolved, filter, pump the filtrate into the crystallization tank, cool to -20°C to -10°C, stir and crystallize for 4 hours, centrifuge Machine filtration, washed 3 times with isopropyl ether, dried, and dried under reduced pressure to obtain 1.87kg retigabine new crystal form D.
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