Hydrate of cyclopeptide compound as well as preparation method and application thereof
A technology of hydrates and compounds, which is applied in the field of pharmaceutical compositions and can solve problems such as poor stability of compounds of formula I
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Embodiment 1
[0181] Preparation of compound I
[0182] Referring to US Pat. No. 5,376,634, the method in Example 1 prepared 153 g of solid powder of the compound shown in Formula I. It uses the Karl Fischer method to measure the moisture content of the compound of formula I to be 3.4%. Take the 2.0g sample obtained above for stability study. The method is as follows: airtight storage at 0-8°C for 6 months, and airtight storage at 25°C for 6 months, and then analyze the impurity content of the samples. The initial impurity content of the compound of formula I was 2.4%, the impurity content of the sample at 0-8°C for 6 months was 3.0%, and the impurity content of the sample at 25°C for 6 months was 4.9%.
Embodiment 2
[0184] Preparation of hydrates A, B, C, D, E containing compounds shown in formula I
[0185] At 50° C., 7.0 g of the solid powder of the compound shown in Formula I prepared in Example 1 was dissolved in a mixed solution of 10 ml of water and 8 ml of n-propanol, and stirred for 30 minutes to completely dissolve the compound shown in Formula I. Adjust the pH to 3.5 with glacial acetic acid, cool the solution to 25°C, the hydrate of the compound represented by formula I precipitates, and continue stirring at 25°C for 5 hours, so that the hydrate of the compound represented by formula I grows gradually. Then slowly add 36ml of n-propanol dropwise, continue stirring at 25°C for 2 hours, and filter to obtain the hydrate of the compound shown in formula I. The hydrate of the compound represented by formula I is vacuum dried at 20°C to 25°C. After drying for 1 hour, 1.0 g of the hydrate was taken and named as hydrate A of the compound shown in formula I, and the mass percent conten...
Embodiment 3
[0192] Preparation of hydrates F, G, H, I, J containing compounds shown in formula I
[0193] At 30° C., 16 g of the compound represented by formula I prepared in Example 1 was dissolved in 90 ml of aqueous solution, and stirred for 2 hours to completely dissolve the compound represented by formula I. Adjust the pH to 2.0 with glacial acetic acid, then slowly add 610ml of ethanol dropwise, the hydrate of the compound represented by formula I precipitates, the solution is cooled to 11°C, and stirred at 11°C for 2 hours. Filtration to obtain the hydrate of the compound represented by formula I. The hydrate of the compound represented by formula I is vacuum dried at 20°C to 25°C. After drying for 0.5 hour, 1.0 g of the hydrate was taken and named as hydrate F of the compound shown in formula I, and the mass percent content of water in F was measured to be 31.2%. The rest of the sample was dried for 0.5 hour, and 1.0 g of the hydrate was taken, named as hydrate G of the compound...
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