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Crystal form b of lurasidone hydrochloride and preparation method thereof
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A technique for the crystal form of alkanediimide hydrochloride, which is applied in the crystal form B of lurasidone hydrochloride and its preparation field, and can solve problems such as crystal forms of compounds not mentioned
Active Publication Date: 2016-07-06
SHANGHAI INST OF PHARMA IND CO LTD +2
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[0004] N-[4-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]-(2R,3R)-2,3-tetramethylene- Butyl]-(1'R, 2'S, 3'R, 4'S)-2,3-bicyclo[2,2,1]heptane diimide hydrochloride, but the application did not mention and the crystal form of the compound
[0005] N-[4-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]-(2R,3R)-2,3-tetramethylene- Butyl]-(1'R, 2'S, 3'R, 4'S)-2,3-bicyclo[2,2,1]heptane diimide hydrochloride, but the application did not mention And the crystal form of the compound, only mentioning that the melting point of the compound is 215°C-217°C
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Embodiment 1
[0029] 10g N-[4-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]-(2R,3R)-2,3-tetramethylene-butyl]- (1'R, 2'S, 3'R, 4'S)-2,3-bicyclo[2,2,1]heptane diimide hydrochloride was added to a mixed solution of 100mL acetone and 36mL water, heated to 40 ℃ dissolve clear, cooling. The obtained solution was left to stand, and the solid was precipitated by filtration, and dried to obtain 5.9 g of a white solid. The obtained product was identified as Form B by X-ray powder diffraction.
Embodiment 2
[0031] 10g N-[4-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]-(2R,3R)-2,3-tetramethylene-butyl]- Add (1'R, 2'S, 3'R, 4'S)-2,3-bicyclo[2,2,1]heptanediimide hydrochloride into 300mL acetone, heat to reflux until dissolved, and continue heating for 1h ,cool down. The resulting solution was stirred overnight, filtered, and dried to obtain 6.8 g of a white solid. The obtained product was identified as Form B by X-ray powder diffraction.
Embodiment 3
[0033] 10g N-[4-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]-(2R,3R)-2,3-tetramethylene-butyl]- Add (1'R, 2'S, 3'R, 4'S)-2,3-bicyclo[2,2,1]heptanediimide hydrochloride into 200mL methanol, heat to reflux until dissolved, and continue heating for 1h ,cool down. The resulting solution was stirred overnight, filtered, and dried to obtain 6.9 g of a white solid. The obtained product was identified as Form B by X-ray powder diffraction.
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Abstract
The invention discloses a crystal form B of N-[4-[4-(1,2-benzisothiazole-3-yl)-1-piperazine]-(2R, 3R)-2,3-tetramethylene-butyl]-(1'R, 2'S, 3'R, 4'S)-2,3-bicyclo[2,2,1], which is characterized in that the crystal form B displays an X-ray powder diffraction pattern having characteristic peaks represented by 2 theta degrees, namely 8.5+ / -0.2, 8.8+ / -0.2, 11.4+ / -0.2, 13.8+ / -0.2, 14.9+ / -0.2, 15.4+ / -0.2, 16.4+ / -0.2, 17.0+ / -0.2, 17.3+ / -0.2, 17.7+ / -0.2, 18.7+ / -0.2, 19.1+ / -0.2, 19.4+ / -0.2, 20.7+ / -0.2, 21.2+ / -0.2, 21.9+ / -0.2, 27.7+ / -0.2, 33.1+ / -0.2, and 35.9+ / -0.2.
Description
technical field [0001] The present invention relates to N-[4-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]-(2R,3R)-2,3-tetramethylene-butyl New crystal of ]-(1'R, 2'S, 3'R, 4'S)-2,3-bicyclo[2,2,1]heptane diimide hydrochloride (lurasidone hydrochloride) Form B and process for its preparation. Background technique [0002] Compound of formula (1) N-[4-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]-(2R,3R)-2,3-tetramethylene -Butyl]-(1'R, 2'S, 3'R, 4'S)-2,3-bicyclo[2,2,1]heptane diimide hydrochloride (common name lurasidone hydrochloride Salt) is a central nervous system drug, suitable for the treatment of schizophrenia and bipolar disorder. [0003] [0004] N-[4-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]-(2R,3R)-2,3-tetramethylene- Butyl]-(1'R, 2'S, 3'R, 4'S)-2,3-bicyclo[2,2,1]heptane diimide hydrochloride, but the application did not mention and the crystal form of the compound. [0005] N-[4-[4-(1,2-benzisothiazol-3-yl)-1-piperazinyl]-(2R,3R)-2,3-tetramethylene- Butyl...
Claims
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