Compound and preparation method and application thereof
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A technology of compound and cyclization reaction, which is applied in the field of biomedicine to achieve the effect of mild conditions, simple reaction operation process, and cheap and easy-to-obtain raw materials
Inactive Publication Date: 2017-07-07
WATERSTONE PHARMA WUHAN
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Problems solved by technology
[0003] However, current efluconazole drugs still need to be improved
Method used
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Embodiment 1
[0044] The preparation of embodiment 1 compound 3
[0045] Add 3.4g NaH (60%) into 400ml DMSO, then add 19.6g trimethyl sulfoxide iodide, stir at room temperature for 1 hour, until no bubbles are generated, with exothermic phenomena during the process, add 20.0g compound 2, and stir at room temperature Stir for one hour, take a sample, and TLC monitoring shows that after the raw material has reacted, add 200 ml of water to dilute, then extract with 1000 ml of ethyl acetate, wash the organic phase with 500 ml of water, wash the organic phase with 500 ml of saturated brine and dry it , concentrated to obtain 19.6g of compound 3 with a yield of 93.2%, which was directly used in the next step.
Embodiment 2
[0046] The preparation of embodiment 2 compound 4
[0047] Add 19g of compound 3 obtained in Example 1 to 190 ml of methanol, then add 285 ml of ammonia water, heat to 60°C and continue the reaction, take a sample after 3 hours, monitor the reaction by thin-layer chromatography, the raw material disappears, and the reaction solution is heated at 40°C Concentrate to remove methanol, add 500 ml of ethyl acetate to extract, wash with water, wash with saturated brine, dry and concentrate to obtain 13.1 g of compound 4 with a yield of 65.0% and a purity of 93.2%.
Embodiment 3
[0048] The preparation of embodiment 3 compound 4
[0049] In addition, compound 4 can also be obtained by the following method: add 5.0 g of compound 3 obtained in Example 1 to 25 ml of methanol, then add 50 ml of ammonia water, heat to 50 ° C and continue the reaction, take a sample after 3 hours, and monitor it by thin layer chromatography After the reaction, the raw materials disappeared. The reaction liquid was concentrated at 40°C to remove methanol, and 200 ml of ethyl acetate was added for extraction, washed with water, washed with saturated brine, dried and concentrated to obtain 2.38 g of compound 4 with a yield of 45.0% and a purity of 92.3%.
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Abstract
The invention provides a compound shown in the formula 1 and a preparation method and application thereof. The method comprises the steps that 1, a compound shown in the formula 2 makes contact with trimethylsulfoxonium iodide to obtain a compound shown in the formula 3; 2, the compound shown in the formula 3 is subjected to a ring-opening reaction to obtain a compound shown in the formula 4; 3, an amino group of the compound shown in the formula 4 is subjected to a ring-closure reaction to obtain a compound shown in the formula 5; 4, the compound shown in the formula 5 is subjected to a de-tetrahydropyrane protection group reaction to obtain a compound shown in the formula 6; 5, the compound shown in the formula 6 is subjected to a molecular inner ring oxidation reaction to obtain a compound shown in the formula 7; 6, the compound shown in the formula 7 makes contact with a compound shown in the formula 8 to obtain the compound shown in the formula 1. According to the method, the compound shown in the formula 1 can be effectively prepared and effectively applied to quality control over an Efinaconazole drug by serving as a reference product.
Description
technical field [0001] The present invention relates to the field of biomedicine. Specifically, the present invention relates to a compound and its preparation method and use. More specifically, the present invention relates to a new impurity of Efluconazole, the synthesis method of the impurity and the preparation method and application of Efluconazole. Use in azole drug detection. Background technique [0002] Efinaconazole (trade name Jublia) was developed by Dow Pharmaceutical. It was approved by the FDA on June 6, 2014, and it is effective for the treatment of fungal diseases in humans and animals. It is clinically used to treat onychomycosis with a 10% solution. [0003] However, current efluconazole drugs still need to be improved. Contents of the invention [0004] The present invention aims to solve one of the technical problems in the related art at least to a certain extent. For this reason, an object of the present invention is to propose a means that can be...
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Application Information
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