Crystal form and preparation method of salt prepared from vinpocetine and perchloric acid
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A technology of vinpocetine and perchloric acid, applied in the direction of organic chemistry, organic chemistry, etc., to achieve the effect of good solubility and stability
Active Publication Date: 2015-11-18
JIANGSU QINGJIANG PHARMA
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[0004] So far there are few relevant reports about the crystal form of the salt of Vinpocetine. In view of this, the technical problem to be solved in the present invention is to overcome the deficiencies in the prior ar...
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Embodiment 1
[0020] At room temperature, add vinpocetine (350mg, 1mmol) into a 100ml Erlenmeyer flask, add 80ml of a mixed solvent of methanol and water (4:1), stir with a magnet for 1 hour, the solution is clear, add 1mmol of perchlorate dropwise Acid, after stirring for 20 minutes, a solid slowly precipitated, then raised the temperature to 40°C, the solid did not melt, then slowly added perchloric acid, when about 3mmol was added, the solid dissolved and cleared, and then slowly volatilized at 40°C, when When it was solid, it was filtered and washed with a small amount of methanol to obtain new salt crystals.
Embodiment 2
[0022] At room temperature, add vinpocetine (350mg, 1mmol) into a 100ml Erlenmeyer flask, add 80ml of a mixed solvent of methanol and water (4:1), stir with a magnet for 1 hour, the solution is clear, add 4mmol of perchlorate dropwise acid, after stirring for 20 minutes, a solid slowly precipitated out, and the solid was filtered to determine that it was a mixed crystal.
Embodiment 3
[0024] At room temperature, vinpocetine (350mg, 1mmol) was added to a 100ml Erlenmeyer flask, 80ml of methanol was added, and after stirring with a magnet for 1 hour, the solution was clear, 1mmol of perchloric acid was added dropwise, and after stirring for 20 minutes, a solid slowly Precipitated, then raised the temperature to 40°C, the solid did not melt, then slowly added perchloric acid, when about 3 mmol was added, the solid still did not melt, filtered, washed with a small amount of methanol to obtain mixed crystals.
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Abstract
The invention relates to a crystal form and a preparation method of a salt prepared from vinpocetine and perchloric acid, and belongs to the technical field of crystal form finding and preparation of medicinal salts. A result of detection through thermogravimetic analysis (TGA), X-ray powder diffraction (P-XRD), X-ray single crystal diffraction (S-XRD), differential scanning calorimetry (DSC) and infrared spectroscopy (IR) shows that the salt is the salt prepared from vinpocetine and perchloric acid. Vinpocetine is an insoluble drug (with the solubility is approximately equal to 5[mu]g/mL and pKa is 7.31), and a result of test of the salt prepared from vinpocetine and perchloric acid shows that the salt has good solubility and stability. The new dosage form of the salt is exploited, and the method lays a foundation for exploitation and application of new dosage forms.
Description
Technical field [0001] The present invention involves a salt crystal and preparation method formed by Changchun Xiding and high chloride. Specifically, the present invention involves the new crystal type and preparation method of the formation of salt forming salt in Changchun Xing and Hemchloric acid.Discover and prepare technology. Background technique [0002] Changchun Setin was first developed by Hungary Gedeonrichter and was listed in 1978.Its pharmacological effects include: increasing cerebral blood flow; promoting the intake and utilization of glucose and oxygen in the brain, increasing ATP, reducing the production of lactic acid during ischemia and hypoxic;Excalities); reduce brain hypoxia damage and protect neurons; enhance the function of dopamine energy, 5throxycinicine, and norepinephrine; prevent the brain, liver, muscle tissue and other parts of ischemic damage; remove free radicals, Anti -fat -resistant peroxidation; enhanced long -term and short -term memory; im...
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