Dapagliflozin intermediate and butynediol mixed crystal and preparation method thereof

By adding seeds of Compound A to the solution of Compound A and butyne glycol, the mixed crystals of dapaliflozin intermediate and butyne glycol are induced to precipitate, which solves the problems of high purity requirements of substrates, high impurity content and low yield before purification in the prior art, and achieves high yield and high purity preparation of Compound A, reducing the preparation cost and production cycle.

CN119708093APending Publication Date: 2025-03-28BEIJING YUEKANGKECHUANG PHARM TECH CO LTD
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Patent Information

Application Number
CN202411906217.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-23
Publication Date
2025-03-28

AI Technical Summary

Technical Problem

In the prior art, when preparing dapaliflozin intermediates, the substrate purity requirements are high, the impurity content is high, and the yield is low before purification, resulting in a long production cost and production cycle.

Method used

The mixed crystal preparation method of dapaliflozin intermediate and butyne glycol is used. By adding seeds of Compound A to the solution of Compound A and butyne glycol, the mixed crystals of Compound A and butyne glycol are induced to precipitate, thereby improving the yield and purity of Compound A.

Benefits of technology

The high yield purification of Compound A was achieved, and the HPLC purity of Compound A could reach more than 99.8%, reducing the preparation cost and production cycle, and improving process robustness and product quality.

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Abstract

The invention provides a dapagliflozin intermediate and butynediol mixed crystal and a preparation method thereof. An X-ray powder diffraction pattern of Cu-K alpha radiation of the mixed crystal has characteristic diffraction peaks corresponding to positions with 2 theta values of 4.9 + / -0.2 degrees, 13.1 + / -0.2 degrees, 13.7 + / -0.2 degrees, 16.4 + / -0.2 degrees, 17.5 + / -0.2 degrees, 19.9 + / -0.2 degrees, 23.4 + / -0.2 degrees, 24.4 + / -0.2 degrees, 28.1 + / -0.2 degrees and 30.0 + / -0.2 degrees. In the preparation of the mixed crystal, the requirement on the purity of the compound A before crystallization is not high, the purification effect on the compound A with the purity of 10% or above is achieved, the product separated out in a mixed crystal form and the compound A are basically separated out in a solid form, the product yield is high, the purity is high, the HPLC purity can reach 99.8% or above, and the product quality is guaranteed.
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