Refining method of tadalafil crystal form I
A technology of tadalafil and purification method, applied in chemical instruments and methods, other chemical processes, organic chemistry and other directions, can solve problems such as easy dispersion, difficulty in further improving the purity of tadalafil form I, and achieve increased binding site, increase the content of reducing groups, and reduce the effect of residues
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[0037] Preparation Example 1
[0038] In the present application, the adsorbent is prepared according to the following method: (1) Mix 4kg of zeolite powder with 8kg of silica sol with a water content of 86%, and leave it for 2 hours to obtain a modified liquid of zeolite powder;
[0039] (2) Mix the zeolite powder modified liquid with 0.8kg of silane coupling agent uniformly to obtain a mixed liquid, heat the mixed liquid in a water bath for 3 hours, then filter the mixed liquid, and dry the solid obtained by filtration to obtain an adsorbent; this step Among them, the silane coupling agent is γ-aminopropyltriethoxysilane.
[0040] As shown in Table 1, the difference between Examples 1-5 is that the weight of the raw materials used to prepare the adsorbent is different.
[0041]
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[0042] Preparation Examples 6-9
[0043] As shown in Table 2, the difference between Preparation Example 3 and Preparation Examples 6-9 is that the moisture content of the silica sol is different.
[0044]
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[0045] Preparation Example 10
[0046] The difference between this preparation example and preparation example 7 is that the silane coupling agent is vinyltriethoxysilane.
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