Acotiamide hydrochloride hydrate crystal form and preparation method thereof
A technology of acotiamide hydrochloride trihydrate and acotiamide hydrochloride, which is applied in the field of medicine, can solve problems such as affecting drug efficacy and differences, and achieves the effects of good repeatability, single crystal form and stable properties
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[0033] Example 1
[0034] Take 3.0 g of acotiamide hydrochloride hydrate and put it into 12.0 g of 20% methanol aqueous solution, and heat under reflux until dissolved. Cool to 20°C and filter. The filter cake was air-dried at 50°C to a moisture content of <8%. It was placed in the air at room temperature until the moisture content was 9.8%-10.5% to obtain 2.31 g of Type A crystalline acotiamide hydrochloride hydrate with a yield of 77.0%.
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[0035] Example 2
[0036] Take 2.0 g of anhydrous acotiamide hydrochloride and put it into 8.0 g of 40% isopropanol aqueous solution, and heat under reflux until dissolved. Cool to 20°C and filter. The filter cake was air-dried at 50°C to a moisture content of <8%. It was placed in the air at room temperature until the moisture content was 9.8%-10.5% to obtain 2.0 g of A-type crystalline acotiamide hydrochloride hydrate with a yield of 90.0%.
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[0037] Example 3
[0038] Take 3.0 g of acotiamide hydrochloride hydrate and put it into 12.0 g of 20% acetonitrile aqueous solution, and heat under reflux until dissolved. Cool to 20°C and filter. The filter cake was air-dried at 50°C to a moisture content of <8%. It was placed in the air at room temperature until the moisture content was 9.8%-10.5% to obtain 2.59 g of A-type crystalline acotiamide hydrochloride hydrate with a yield of 86.3%.
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