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A kind of preparation technology of lobeline hydrochloride

A lobeline hydrochloride and preparation technology, which is applied in the field of drug synthesis, can solve problems such as difficult compliance of material indicators, and achieve the effects of increased yield and simple operation

Active Publication Date: 2017-11-21
双鹤药业(商丘)有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield is about 65%, and the relevant substance indicators of the product are difficult to meet the indicators of the Chinese Pharmacopoeia 2010 Edition

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of preparation technology of lobeline hydrochloride, comprises the steps:

[0022] (1) Under stirring, 20 g of levo-lobeline, 40 g of absolute ethanol and 120 g of methyl tert-butyl ether were sequentially added to the reactor at room temperature, and mixed uniformly to prepare mixture a;

[0023] (2) Under stirring, first add 14g of 20% hydrogen chloride-ethanol solution by mass percentage to the mixture a obtained in step (1), then start to heat slowly at a heating rate of 2~4°C / min, and stop when reflux occurs Raise the temperature, keep it warm for 1 hour, stop stirring; then lower the temperature to 0~5°C, crystallize for 4~6 hours, and filter to obtain a filter cake;

[0024] (3) Wash the filter cake obtained in step (2) with methyl tert-butyl ether and absolute ethanol once respectively, collect the material; blow and dry at a temperature of 45~60°C to obtain a white crystalline powder that is product.

[0025] The white crystalline powder obtained in th...

Embodiment 2

[0027] A kind of preparation technology of lobeline hydrochloride, comprises the steps:

[0028] (2) Under stirring, 20 g of levo-lobeline, 40 g of absolute ethanol and 160 g of methyl tert-butyl ether were sequentially added to the reactor at room temperature, and mixed uniformly to prepare mixture a;

[0029] (2) Under stirring, first add 14g of 20% hydrogen chloride-ethanol solution by mass percentage to the mixture a obtained in step (1), then start to heat slowly at a heating rate of 2~4°C / min, and stop when reflux occurs Raise the temperature, keep it warm for 1 hour, stop stirring; then lower the temperature to 0~5°C, crystallize for 4~6 hours, and filter to obtain a filter cake;

[0030] (4) Wash the filter cake obtained in step (2) with methyl tert-butyl ether and absolute ethanol once respectively, collect the material; blow and dry at a temperature of 45~60°C to obtain a white crystalline powder that is product.

[0031] The white crystalline powder obtained in th...

Embodiment 3

[0033] A kind of preparation technology of lobeline hydrochloride, comprises the steps:

[0034] (3) Under stirring, 20 g of levo-lobeline, 40 g of absolute ethanol and 240 g of methyl tert-butyl ether were sequentially added to the reactor at room temperature, and mixed uniformly to prepare mixture a;

[0035] (2) Under stirring, first add 14g of 20% hydrogen chloride-ethanol solution by mass percentage to the mixture a obtained in step (1), then start to heat slowly at a heating rate of 2~4°C / min, and stop when reflux occurs Raise the temperature, keep it warm for 1 hour, stop stirring; then lower the temperature to 0~5°C, crystallize for 4~6 hours, and filter to obtain a filter cake;

[0036] (5) Wash the filter cake obtained in step (2) with methyl tert-butyl ether and absolute ethanol once respectively, collect the material; blow and dry at a temperature of 45~60°C to obtain a white crystalline powder that is product.

[0037] The white crystalline powder obtained in th...

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PUM

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Abstract

The invention relates to a preparation technique of lobeline hydrochloride, which comprises the following steps: sequentially adding levo-lobeline, anhydrous ethanol and methyl tert-butyl ether into a reactor at room temperature under stirring conditions, and uniformly mixing to obtain a mixture a; adding a 10-25 wt% hydrogen chloride-ethanol solution into the mixture a, starting slowly heating at the heating rate of 2-4 DEG C / minute, stopping heating when reflux appears, keeping the temperature to react for 0.5-2 hours, and stopping stirring; cooling to 0-5 DEG C, crystallizing for 4-6 hours, and filtering to obtain a filter cake; sequentially washing the filter cake with methyl tert-butyl ether and anhydrous ethanol, and collecting the material; and carrying out forced air drying at 45-60 DEG C to obtain the white crystalline powder product. The method enhances the yield and lowers the cost. Various indexes of the product conform to Chinese Pharmacopoeia 2010 Edition and Chinese Pharmacopoeia 2015 Edition.

Description

technical field [0001] The invention belongs to the technical field of drug synthesis, and in particular relates to a preparation process of lobeline hydrochloride. Background technique [0002] Lobeline hydrochloride is white crystal or granular powder, odorless and bitter; the aqueous solution is weakly acidic. This product is soluble in ethanol or chloroform and dissolved in water. [0003] Lobeline hydrochloride can selectively excite carotid body chemoreceptors, reflexively excite the respiratory center, and large doses can also directly excite the respiratory center. It can stimulate carotid sinus and aortic body chemoreceptors (both N1 receptors), and reflexively excite the respiratory center to accelerate breathing, but has no direct excitatory effect on the respiratory center. It also has a reflex excitatory effect on the vagus nerve center and vasomotor center at the same time; it excites the autonomic ganglion first and then blocks it. Neonatal asphyxia, inhala...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D211/32
CPCC07D211/32
Inventor 朱圣南孙韶军
Owner 双鹤药业(商丘)有限责任公司