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Levosulpiride compound and preparation method thereof

A levosulpiride compound technology, applied in the field of levosulpiride compound and its preparation, can solve the problems of low molar yield, long production cycle, and unstable products, etc., and achieve the goal of reducing production cost, increasing reaction yield, and shortening the production cycle Effect

Active Publication Date: 2013-12-04
QIDONG HUATUO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production of levosulpiride includes chemical synthesis method and resin column separation method, both of which have disadvantages such as low molar yield, long production cycle, high production cost, difficult industrialization, unstable product, and short validity period.

Method used

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  • Levosulpiride compound and preparation method thereof
  • Levosulpiride compound and preparation method thereof
  • Levosulpiride compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Take 20g of sulpiride, put it in an ultrasonic chemical reactor, add 82g of methanol, 16g of N,N-dimethylformamide, stir for 30 minutes, add 2g of ferric oxide fine powder, select the ultrasonic frequency of 32.45 kHz, keep for 2 hours, filter, Discard the filter residue, add 50 g of water, stir for 30 minutes, cool the filtrate to 2°C, select an ultrasonic frequency of 40kHz, vacuum degree of 0.02MPa, keep for 2 hours, crystallize, filter out, and vacuum dry at 50°C to obtain 21.38g of levosulpiride dihydrate , and the molar yield was 96.72%.

specific Embodiment 2

[0026] Take 20g of sulpiride, put it in an ultrasonic chemical reactor, add 84g of methanol, 18g of N,N-dimethylformamide, stir for 30 minutes, add 2g of ferric oxide fine powder, select the ultrasonic frequency of 32.45 kHz, keep for 2 hours, filter, Discard the filter residue, add 50g of water, stir for 30 minutes, cool the filtrate to 4°C, select an ultrasonic frequency of 50kHz, vacuum degree of 0.04MPa, keep it for 2 hours, crystallize, filter out, and vacuum dry at 60°C to obtain 21.47g of levosulpiride dihydrate , and the molar yield was 97.13%.

specific Embodiment 3

[0028] Take 20kg of sulpiride, put it in an ultrasonic chemical reactor, add 83kg of methanol, 17kg of N,N-dimethylformamide, stir for 30 minutes, add 2kg of ferric oxide fine powder, select the ultrasonic frequency of 32.45 kHz, keep for 2 hours, filter, Discard the filter residue, add 50kg of water, stir for 30 minutes, cool the filtrate to 3°C, select an ultrasonic frequency of 45kHz, vacuum degree of 0.03MPa, keep for 2 hours, crystallize, filter out, and vacuum dry at 55°C to obtain 21.66kg of levosulpiride dihydrate , and the molar yield was 98.0%.

[0029] The above examples illustrate that levosulpiride dihydrate can be made by adopting the extreme conditions and optimized conditions of the embodiment of the present invention, and the levosulpiride obtained in Example 3 is used to investigate the actual effect of the present invention below:

[0030] 1 The production cycle of levosulpiride prepared by the present invention is compared with the production cycle of levos...

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Abstract

The invention discloses a levosulpiride compound and a preparation method of the levosulpiride compound. The method is characterized in that methyl alcohol and N,N-dimethylformamide in prescribed proportion are adopted as solvents, sulpiride is resolved under the ultrasound condition to achieve turnover of dextroisomer, low temperature vacuum ultrasound is adopted for crystallization, and novel levosulpiride dehydrate and the preparation method of the levosulpiride dehydrate are obtained. The levosulpiride compound and the preparation method are moderate in resolution condition and easy to industrialize, improves the product yield and purity, shortens the resolution time and reduces cost, product stability is good, the validity period is prolonged, and a satisfied effect is obtained.

Description

technical field [0001] The invention relates to the field of chemical medicine preparation, in particular to a levosulpiride compound and a preparation method thereof. Background technique [0002] Sulpiride is an ideal antipsychotic drug for the treatment of schizophrenia, and also for intractable vomiting, peptic ulcer and dizziness and headache after traumatic brain injury. Sulpiride is a racemic form, in which the L-form plays a major role, and the D-form has almost no effect, but increases the toxic and side effects of the drug. However, the properties of the two are very similar and it is difficult to separate them. At present, the production of levosulpiride includes chemical synthesis and resin column separation methods, both of which have disadvantages such as low molar yield, long production cycle, high production cost, difficult industrialization, unstable product, and short validity period. In my long-term synthesis and resolution experiments of levosulpiride, I...

Claims

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Application Information

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IPC IPC(8): C07D207/09
Inventor 孙威
Owner QIDONG HUATUO PHARMA
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