Method for preparing A-type crystal of Atazanavir disulfate

A technology of bisulfate and atazanavir is applied in the field of preparation of type A crystal of atazanavir bisulfate, which can solve the problems of harsh speed requirements, poor process stability and high purity requirements of concentrated sulfuric acid, and is convenient for industrial production. , The effect of high crystal purity and high product yield
CN105859611AInactive Publication Date: 2016-08-17SHANGHAI SHYNDEC PHARMA HAIMEN CO LTD +2
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
SHANGHAI SHYNDEC PHARMA HAIMEN CO LTD
Publication Date
2016-08-17
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention discloses a method for preparing an A-type crystal of Atazanavir disulfate. The method comprises the following steps that a, Atazanavir free alkali is placed in ethyl alcohol, the mixture is stirred at room temperature, then concentrated sulfuric acid is added dropwise, the reaction liquid is heated and stirred, then an inert solvent is added, cooling and crystallization are carried out, drying is carried out after filtering, and an Atazanavir ethyl alcohol compound E-type crystal is obtained, wherein the molar concentration of concentrated sulfuric acid is preferably 15 mol / L to 18.4 mol / L; b, the Atazanavir ethyl alcohol compound E-type crystal obtained in the step a is placed in acetone, heating, refluxing and stirring are carried out, drying is carried out after cooling and filtering, and the A-type crystal of Atazanavir disulfate is obtained. According to the crystal transformation preparation method, the operability of the process is improved, the external properties of the product are improved, and the quality and purity of the product are improved.
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Description

technical field

[0001] The invention relates to the technical field of medicinal chemistry, in particular to a method for preparing atazanavir bisulfate type A crystals. Background technique

[0002] Atazanavir Sulfate, trade name Reyataz, was developed by Bristol-Myers Squibb and was approved by the US FDA in June 2003. It is mainly used in combination with other antiretroviral drugs to treat HIV infection .

[0003] Atazanavir sulfate or atazanavir bisulfate, chemical name is (3S, 8S, 9S, 12S)-3,12-bis(1,1-dimethylethyl)-8-hydroxy-4, 11-Dioxo-9-(phenylmethyl)-6-[[4-(2-pyrimidine)phenyl]methyl]-2, 5,6, 10, 13-pentaazatetradecanedioic acid Dimethyl sulfate (1:1), the structure is as follows:

[0004] .

[0005] Atazanavir hydrogen sulfate exists in various crystal forms including hydrates and solvates. Its pharmaceutical crystal form is anhydrous, non-solvated crystal form A (US 6087383 reported its crystal form and preparation method for the first time).

[0006] US...

Claims

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