Method for preparing voriconazole resolution intermediate
A technology of voriconazole and voricon, which is applied in the field of preparing voriconazole intermediates, can solve problems such as difficult separation, low production capacity, and increased production costs, and achieve the effects of huge market prospects, strong antibacterial efficacy, and broad antifungal spectrum
Active Publication Date: 2017-02-22
ZHEJIANG HUAHAI PHARMA CO LTD
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Problems solved by technology
[0012] 1. The two solvents, methanol and acetone, have relatively close boiling points and strong volatility, so it is difficult to separate them. Therefore, the solvent recovery of split products is a big problem, which increases production costs and is not environmentally friendly. production requirements
[0013] 2. In the splitting process, the amount of splitting solvent used is very large, and the production capacity is low, which seriously affects the large-scale production of splitting products
Method used
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Experimental program
Comparison scheme
Effect test
Embodiment 1
[0020] Voriconazole racemate (9g), L-camphorsulfonic acid (6g), acetone (150mL), water (30mL), heated up to 50°C, the solution was clear, naturally cooled to 0°C, stirred at 0°C for 2 hours, filtered, HPLC detection, ee%=99.3%, yield 30.1%.
Embodiment 2
[0022] Voriconazole racemate (9g), L-camphorsulfonic acid (6g), acetone (150mL), water (15mL), heated up to 50°C, the solution was clear, naturally cooled to 25°C, stirred at 25°C for 2 hours, filtered, HPLC detection, ee%=99.7%, yield 36.6%.
Embodiment 3
[0024] Voriconazole racemate (15g), L-camphorsulfonic acid (10g), acetone (150mL), water (15mL), heated up to 50°C, the solution was clear, naturally cooled to 20°C, stirred at 20°C for 2 hours, filtered, HPLC detection, ee%=99.7%, yield 40.4%.
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Abstract
The invention provides a new method for preparing voriconazole levorotation camphor sulfonate. The method comprises the following steps: dissolving a voriconazole raceme and levorotation camphor sulfonic acid in a mixed solvent consisting of water and acetone, performing cooling crystallization, and performing filtration and drying to obtain the voriconazole levorotation camphor sulfonate. According to the method provided by the invention, the production cost is effectively reduced by adjusting a resolution solvent.
Description
technical field [0001] The invention relates to a method for preparing a voriconazole intermediate. Background technique [0002] Voriconazole (Voriconazole, VRC, UK109496) is a new type of antifungal drug synthesized by Pfizer based on fluconazole. It is mainly used for patients with progressive and fatal immunocompromised patients. Because voriconazole has a wide antifungal spectrum, strong antibacterial efficacy, and good safety, and the demand for antifungal drugs in the domestic market is growing rapidly, the market prospect is huge. [0003] Voriconazole, its chemical name is: (2R,3S)-2-(2,4-difluorophenyl)-3-(5-fluoropyrimidin-4-yl)-1-(1H-1,2,4- Triazol-1-yl)-2-butanol, the structural formula is as shown in formula I: [0004] [0005] Voriconazole racemate is an important intermediate, chemical name: (2R,3S / 2S,3R)-2-(2,4-difluorophenyl)-3-(5-fluoropyrimidine-4- Base)-1-(1H-1,2,4-triazol-1-yl)-2-butanol, the structural formula is as shown in Formula II: [0006...
Claims
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IPC IPC(8): C07D403/06C07B57/00
CPCC07B57/00C07D403/06C07B2200/07C07C303/22C07C309/19C07C2603/66C07B2200/13
Inventor 黄虎黄文锋涂国良徐中明吴强晖孟昭旸方玉玲
Owner ZHEJIANG HUAHAI PHARMA CO LTD