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Purification method of haloperidol

A technology of haloperidol and a purification method, applied in the direction of organic chemistry, which can solve the problems of difficult removal of dimerization impurities and inability to obtain active drug molecules with qualified purity, and achieve the effect of high product yield

Active Publication Date: 2020-05-22
SHANGHAI XUDONG HAIPU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The second step reaction of this route is easy to produce multiple impurities, especially dimeric impurities are difficult to remove, and active drug molecules with qualified purity cannot be obtained, as shown in the following formula II:

Method used

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  • Purification method of haloperidol
  • Purification method of haloperidol
  • Purification method of haloperidol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Example 1 Preparation of crude haloperidol (170826 batches, dimerization impurity content: 0.38w / w%)

[0021]

[0022] Add starting material III (10.01g), intermediate (28.40g), sodium carbonate (10.01g), potassium iodide (3.92g) and methyl isobutyl ketone (200mL) into a 500mL reaction flask, heat up to 130°C, heat and stir , reacted for 6 hours (HPLC detection of starting material III<5.0%), cooled to 50°C, added water (100mL) and stirred for 0.5h, separated the organic layer, and the organic layer continued to drop to 10-20°C for crystallization, filtered, and used for filter cake A small amount of methyl isobutyl ketone was washed, and air-dried at 55°C to obtain 14.7 g of the product, with a yield of 82.7%.

Embodiment 2

[0023] Example 2 Preparation of crude haloperidol (170808 batches, dimerization impurity content: 0.57w / w%)

[0024] Add starting material III (20.1g), intermediate (57.0g), potassium iodide (0.80g), sodium carbonate (20.0g) and methyl isobutyl ketone (600mL) into the reaction flask, heat up and stir, and react at 130°C for 6 hours (HPLC detection starting material III<5.0%), cooled to 50°C, added water (200mL) and stirred for 0.5h, separated the organic layer, and the organic layer continued to drop to 10°C-20°C for crystallization, filtered, and the filter cake was washed with a small amount of formazan Washed with isobutyl ketone and air-dried at 55°C to obtain 30.0 g of the product with a yield of 84.1%.

Embodiment 3

[0025] The refining of embodiment 3 haloperidol crude product

[0026] Add 1.0g of the crude product (batch 170821-2) and 10mL of absolute ethanol to a 100mL reaction bottle, stir and heat to 70°C, after dissolving, add 2mL of water dropwise, the system is turbid, cool down to 10°C-20°C, filter, 55°C Air-dried to obtain 0.80 g, yield 80.0%.

[0027] In this example, the refining solvent: ethanol / water, the purity of haloperidol in the crude product is 89.37%, and 99.12% after purification, and the content of dimer impurities is about 0.4w / w%, indicating that the removal of dimer impurities is not significant, and other impurities Has been visibly removed.

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Abstract

A method for purifying haloperidol, first dissolving the prepared crude haloperidol in hot DMSO solution, filtering to remove dimer impurities insoluble in DMSO, and obtaining haloperidol with qualified dimer impurity content alcohol. In the method for purifying haloperidol provided by the present invention, the crude product of haloperidol is added into a hot DMSO solution to efficiently remove the dimerized impurities generated during the synthesis, so that the dimerized impurities of the obtained haloperidol The content is less than 0.05w / w%.

Description

technical field [0001] The invention relates to a method for preparing butyrophenone compounds, in particular to a method for purifying haloperidol, which improves the purity of the product. Background technique [0002] Haloperidol acute and chronic schizophrenia and mania. Intramuscular injection of this product can quickly control agitation, hostility and aggressive behavior, and can also be used for brain organic mental disorders and senile mental disorders. [0003] Synthetic process route is shown in following formula I: [0004] [0005] The second step reaction of this route is easy to produce multiple impurities, especially dimeric impurities are difficult to remove, and active drug molecules with qualified purity cannot be obtained, as shown in the following formula II: [0006] [0007] The commonly used refining method is to remove the impurity by dissolving in an organic solvent and then crystallizing. Contents of the invention [0008] The object of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/52
CPCC07D211/52
Inventor 陈小林杨易可占娅锋高鹏飞孙晔
Owner SHANGHAI XUDONG HAIPU PHARMA
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