Crystal form, preparation method and application of prostaglandin analogue
一种晶型、药物的技术，应用在化学制药领域，能够解决前列腺素类化合物稳定性差等问题
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[0050] The preparation method of compound I crystal form A
[0051] The present invention also provides a preparation method of crystal form A of the compound represented by formula I.
[0052] In one embodiment provided by the invention, the preparation method of the crystal form A of the compound of formula I comprises the following steps:
[0053] (1) Mix the crude product of the compound shown in formula I with solvent 1 to obtain solution 1; the solvent 1 is selected from the group consisting of methanol, acetonitrile, ethyl acetate, methyl acetate, isopropyl acetate, and / or or tert-butyl acetate;
[0054] (2) Cool down the temperature of solution 1 or add solvent 2 and stir to precipitate crystal form A of the compound of formula I.
[0055] In step (1), the mixing should be performed below the boiling point of solvent 1, preferably at 0-80°C; preferably at 20-50°C; more preferably at 30-50°C.
[0056] In step (1), the mixing ratio (weight to volume ratio) of the crud...
Embodiment 1
[0082] Preparation of crude compound I
[0083] With reference to the preparation method reported in the document J.Org.Chern.2004, 69, 1890-1902, (1R, 2R, 3aS, 9aS)-2,3,3a,4,9,9a-hexahydro-1-[( 3S)-3-Hydroxyoctyl]-1H-phenyl[f]indene-2,5-diol was used as the starting material, and 41 g of crude compound I was obtained without purification.
Embodiment 4
[0089] Preparation of compound I crystal form A
[0090] In a 25ml eggplant-shaped bottle, add the compound I crude product (1.0g) and methanol (1.0ml) obtained in Example 1, warm up to 30°C and dissolve to form a homogeneous solution, then slowly add pure water (0.6ml), and cool down to Stir at 5°C for 10 h, filter, wash with 10% aqueous methanol at 5°C for 2-3 times, and dry to obtain 0.91 g of crystalline solid. X-ray powder diffraction pattern see figure 1 , differential scanning calorimetry (DSC) chart see figure 2 , see the infrared spectrum image 3 , HPLC purity 99.90%. Organic residue: methanol 0.04% (mass yield: 91%)
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