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Preparation method of high-purity mepivacaine hydrochloride

A technology of mepivacaine hydrochloride and mepivacaine, which is applied in the field of biomedicine, can solve problems such as time-consuming and labor-consuming, impurity removal, loss of yield and high cost, and achieve the effect of simple operation and improved purity

Pending Publication Date: 2022-06-07
MAXENMED GUANGZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Impurities (Formula 6), (Formula 7), and (Formula 8) in the process cannot be well removed by recrystallization. Time-consuming and labor-intensive, but also loss of yield leads to higher cost

Method used

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  • Preparation method of high-purity mepivacaine hydrochloride
  • Preparation method of high-purity mepivacaine hydrochloride
  • Preparation method of high-purity mepivacaine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] A method for preparing high-purity mepivacaine hydrochloride, comprising the following steps:

[0048] S1, Preparation of mepivacaine crude products:

[0049] S11, 14kg of anhydrous formic acid was added to the 50-liter glass reactor, 3.8kgN- (2',6'-xylphenyl)-2-piperidinecarboxamide was added in batches at 20 °C, 50 minutes of heat preservation and stirring, 1.5kg of paraformaldehyde was added, heated to 95 °C, insulation reaction for 10 hours, after the reaction was completed, cooled to 25 °C, added 4N hydrochloric acid 9.95kg, and then reduced pressure to concentrate and remove the solvent;

[0050] S12, remove the solvent and dissolve with 10kg of water stirring; Adjust pH ≥13 with 20% sodium hydroxide solution at 20 °C, filter, wash the filter cake with 2 kg of water, collect the filter cake, vacuum dry for 12 hours (vacuum degree is -0.08MPa, temperature is 55 °C), give crude mepivacaine 3.67kg, yield 91%, mp 148-152 °C; See high performance liquid chromatography Figu...

Embodiment 2

[0056] A method for preparing high-purity mepivacaine hydrochloride, comprising the following steps:

[0057] S1, Preparation of mepivacaine crude products:

[0058] S11, 280g of anhydrous formic acid was added to a 1-liter glass reactor, 76gN- (2',6'-xylphenyl)-2-piperidinecarboxamide was added in batches at 20 °C, stirred for 50 minutes, paraformaldehyde was added 30g, heated to 95 °C, insulation reaction for 10 hours, after the reaction was completed, cooled down to 25 °C, added 4N hydrochloric acid 200g, and then concentrated to remove the solvent under reduced pressure;

[0059] S12, remove the solvent with 200g of water stirred to dissolve; Adjust pH ≥13 with 20% sodium hydroxide solution at 20 °C, filter, wash the filter cake with 40 g of water, collect the filter cake, vacuum dry for 12 hours (vacuum degree -0.08MPa, temperature is 55 °C), to give mepivacaine crude product 73.6 g, yield 92%, mp 148-152 °C.

[0060] Preparation of S2, high-purity mepivacaine hydrochloride: ...

Embodiment 3

[0065] A method for preparing high-purity mepivacaine hydrochloride, comprising the following steps:

[0066] S1, Preparation of mepivacaine crude products:

[0067] S11, 1.4kg of anhydrous formic acid was added to a 5-liter glass reactor, 380gN- (2',6'-xylphenyl)-2-piperidinecarboxamide was added in batches at 20 °C, stirred for 50 minutes, added paraformaldehyde 150g, heated to 95 °C, insulation reaction for 10 hours, after the reaction, cooled down to 25 °C, added 4N hydrochloric acid 995g, and then reduced pressure to remove the concentrated solvent;

[0068] S12, remove the solvent and stir it to dissolve with 1kg of water; Adjust pH ≥13 with 20% sodium hydroxide solution at 20 °C, filter, wash the filter cake with 200g of water, collect the filter cake, vacuum dry for 12 hours (vacuum degree of -0.08MPa, temperature of 55 °C), to give mepivacaine crude product 0.372kg, yield 91.8%, mp 148-152 °C.

[0069]Preparation of S2, high-purity mepivacaine hydrochloride:

[0070] S21、...

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Abstract

The invention discloses a preparation method of high-purity mepivacaine hydrochloride, and belongs to the technical field of biological medicines.The preparation method of the high-purity mepivacaine hydrochloride comprises the following steps that a mepivacaine crude product reacts with tartaric acid to generate mepivacaine tartrate; the preparation method comprises the following steps: dissolving mepivacaine tartrate in water, adding a sodium hydroxide solution, uniformly stirring, and filtering to obtain a high-purity mepivacaine solid; and dissolving the high-purity mepivacaine solid in an organic solvent, filtering, taking filtrate, introducing dry hydrogen chloride gas into the filtrate, stirring to form salt, filtering, and drying to obtain the high-purity mepivacaine hydrochloride. According to the preparation method, various impurities generated in the synthesis process of mepivacaine hydrochloride can be effectively removed, so that the purity of mepivacaine hydrochloride is improved, the purity of mepivacaine hydrochloride is larger than 99.9%, and the total yield of the product is larger than 85% when mepivacaine crude products are used for calculating the total yield of the product.

Description

Technical field [0001] The present invention relates to the field of biomedical technology, specifically to a high purity method for the preparation of mepivacaine hydrochloride. Background [0002] Methylpivacaine hydrochloride (1 Mepivacaine Hydrochloride), also known as carbocaine hydrochloride, chemical name: 1-methyl-N- (2,6-xylphenyl)-2-piperidinecarboxamide hydrochloride, which is an amide local anesthetic, the chemical structure is similar to lidocaine, but its onset speed, strong anesthesia effect, stable nature, toxicity and small side effects, etc., has been widely used in Europe, America, Japan and South Korea and other countries, its structural formula 1 shows: [0003] [0004] N- (2',6'-dimethylphenyl)-2-piperidinecarboxamide (structural formula as shown in formula 2) is an important intermediate for the synthesis of this similar anesthetic, the intermediate synthesis route such as Scheme1, the process of synthesis (formula 2) will inevitably produce self-condens...

Claims

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Application Information

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IPC IPC(8): C07D211/60
CPCC07D211/60
Inventor 郭淑儿覃志君
Owner MAXENMED GUANGZHOU
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