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A kind of method that reclaims articaine hydrochloride or its intermediate product from synthetic mother liquor

A technology for synthesizing articaine hydrochloride and mother liquor, applied to medical preparations containing active ingredients, pharmaceutical formulas, drug combinations, etc., can solve problems such as waste, high cost, and difficult processing, and achieve the effect of reducing waste

Active Publication Date: 2019-10-25
蚌埠丰原涂山制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Yet it is a kind of waste that the mother liquor of articaine hydrochloride only reclaims the concentrated solution after the solvent and makes waste liquid treatment, because it contains many useful articaine hydrochloride intermediate product compounds 3 and articaine hydrochloride after all; Concentrated viscous liquid, if it is treated as waste liquid, it is very difficult and expensive

Method used

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  • A kind of method that reclaims articaine hydrochloride or its intermediate product from synthetic mother liquor
  • A kind of method that reclaims articaine hydrochloride or its intermediate product from synthetic mother liquor
  • A kind of method that reclaims articaine hydrochloride or its intermediate product from synthetic mother liquor

Examples

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Effect test

Embodiment 1

[0038] Produce a batch of intermediate product 1 (4-methyl-3[[1-oxo-2-(chloro)propyl]amino]-2-thiophene carboxylate methyl ester) according to the flow process and production requirements: wherein raw materials (3 -Amino-4-methyl-thiophene-2-carboxylic acid methyl ester) input amount is 29kg, the theoretical output intermediate product 1 is 44.3kg, the actual production obtains the qualified intermediate product 1 is 29.2kg, and the yield is 65.9%. Collect 115kg of the mother liquor produced in the production of intermediate product 1 in this step, set the water bath temperature at 75°C and concentrate in vacuum until no obvious fraction appears to obtain 56kg of viscous feed solution, add 50kg of methanol and heat to reflux for dissolution, then cool down to 2°C and discharge to obtain Viscous material liquid (black in color, no obvious crystallization). The above viscous feed liquid was reworked and re-concentrated in vacuum until there was no obvious fraction, and 110 kg of...

Embodiment 2

[0040]Produce a batch of intermediate product 1 (4-methyl-3[[1-oxo-2-(chloro)propyl]amino]-2-thiophene carboxylate methyl ester) according to the flow process and production requirements: wherein raw materials (3 -Amino-4-methyl-thiophene-2-carboxylic acid methyl ester) input amount is 29kg, the theoretical output intermediate product 1 is 44.3kg, the actual production obtains the qualified intermediate product 1 is 30.1kg yield 67.9%. Collect 112kg of mother liquor produced in the production of intermediate product 1 in this step, set the water bath temperature at 71°C and concentrate in vacuum until no obvious fraction appears to obtain 52.5kg of viscous feed solution, add 50kg of methanol and heat to reflux to dissolve, then cool down to 2°C and discharge Viscous feed liquid (black in color, no obvious crystallization) was obtained. The above viscous feed liquid was reworked and re-concentrated in vacuum until there was no obvious fraction, and 110 kg of dichloromethane and...

Embodiment 3

[0042] Produce a batch of intermediate product 1 (4-methyl-3[[1-oxo-2-(chloro)propyl]amino]-2-thiophene carboxylate methyl ester) according to the flow process and production requirements: wherein raw materials (3 -Amino-4-methyl-thiophene-2-carboxylic acid methyl ester) input amount was 29kg, the theoretical output of compound 3 was 44.3kg, and the actual production obtained qualified intermediate product 1 was 27.2kg with a yield of 61.4%. Collect 117kg of mother liquor produced by the production of intermediate product 1 in this step, set the water bath temperature at 73°C and concentrate in vacuum until no obvious fraction appears to obtain 58kg of viscous feed solution, add 110kg of dichloromethane and 100kg of saturated saline, stir for 20 minutes, and let stand for 30 Minute layering. The organic layer was collected and the aqueous layer was discarded. Control the temperature of the water bath at 60-65°C and concentrate in vacuum until no obvious fraction appears to ob...

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Abstract

The invention relates to a method for recovering articaine hydrochloride or intermediate products thereof in self-synthetic mother liquor. The method comprises the following steps: (1) concentrating synthetic mother liquor of articaine hydrochloride or intermediate products thereof, adding a weakly polar organic solvent and an inorganic saline solution, fully stirring, standing and collecting an organic phase; and (2) concentrating the organic phase obtained in the step (1), adding a strongly polar organic solvent for fully dissolving, cooling, and crystallizing, thereby obtaining the product. The synthetic mother liquor of articaine hydrochloride or intermediate products thereof is synthetic mother liquor enriched in the intermediate products or articaine hydrochloride produced by each step in the process of preparing a final product articaine hydrochloride by taking 3-amino-4-methyl-thiophene-2-carboxylic acid methyl ester as a raw material. According to the method provided by the invention, the recyclable target products in the mother liquor are recovered to the greatest degree, the waste of materials is reduced, and the waste liquor treatment cost and environmental pollution can be reduced.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a method for recovering articaine hydrochloride or its intermediate product from synthesis mother liquor. Background technique [0002] Articaine hydrochloride, molecular formula: C 13 h 20 N 2 o 3 S, molecular weight: 320.8, structural formula as follows: [0003] [0004] Articaine hydrochloride is an amide local injection anesthetic, which can block the nerve conduction along the nerve fibers at the injection site and act as a local anesthetic. Compared with other local anesthetics, the main feature of articaine hydrochloride is the onset time of anesthesia Fast; strong tissue infiltration, no block anesthesia; high anesthesia efficiency, large safety range, appropriate duration of anesthesia; low incidence of allergies, less impact on the cardiovascular system, and low toxic and side effects. Particularly suitable for surgical procedures involving o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D333/38A61K31/381A61P23/02
CPCC07D333/38
Inventor 张祖杨夏继祥李保琴单永继许祥雷王大伟胡志国
Owner 蚌埠丰原涂山制药有限公司