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Preparation method of ropivacaine hydrochloride impurities

A technology for ropivacaine hydrochloride and impurities, which is applied in the field of preparation of ropivacaine hydrochloride impurities, can solve the problems of the undisclosed preparation method of ropivacaine hydrochloride impurities, and achieve high purity, high yield and low cost Effect

Pending Publication Date: 2020-11-13
GUANGDONG JIABO PHARM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But also the preparation method of impurity in the synthetic process of ropivacaine hydrochloride is not disclosed at present

Method used

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  • Preparation method of ropivacaine hydrochloride impurities
  • Preparation method of ropivacaine hydrochloride impurities
  • Preparation method of ropivacaine hydrochloride impurities

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preparation example Construction

[0028] The invention provides a method for preparing impurities of ropivacaine hydrochloride, the chemical structural formula of the impurities of ropivacaine hydrochloride is shown in formula I;

[0029]

[0030] The preparation method of the impurity of ropivacaine hydrochloride is obtained by mixing and purifying 2,6-dimethylaniline, Vilsmeier-Haack acid halide reagent and N,N-dimethylformamide.

[0031] Further, the method includes the following steps:

[0032] (1) 2,6-dimethylaniline, Vilsmeier-Haack acid halide reagent and N,N-dimethylformamide are mixed and stirred for reaction;

[0033] (2) adding water to the reaction system after the reaction in step (1) to quench and adjust the pH value to be not less than 6 and extract with an organic solvent;

[0034] (3) concentration and purification to obtain the ropivacaine hydrochloride impurity.

Embodiment 1

[0036] A kind of preparation method of ropivacaine hydrochloride impurity as the embodiment of the present invention, described method comprises the following steps:

[0037] (1) Mix and stir 5.2g of 2,6-dimethylaniline (0.043mol), 13.0g of phosphorus oxychloride (0.085mol) and 40mL of N,N-dimethylformamide until the reaction is completed, and pass through the point The plate method judges the end of the reaction;

[0038] (2) adding water to the reaction system after the reaction in step (1) to quench and adjust the pH value to 12 with sodium hydroxide and extract with toluene;

[0039] (3) The organic phases were combined, spin-dried, concentrated to dryness after passing through the column to obtain a white solid powder.

[0040] After determination, the present embodiment prepares 4.0 g of white solid powder with a purity of 99.0%. After mass spectrometry and nuclear magnetic detection, the result is 1 H-NMR (CDCl 3 , 400MHz): δ2.17(6H,s), 2.99(6H,s), 6.60~7.34(4H,m); m...

Embodiment 2

[0042] A kind of preparation method of ropivacaine hydrochloride impurity as the embodiment of the present invention, described method comprises the following steps:

[0043] (1) 5.2 g of 2,6-dimethylaniline (0.043 mol), 13.0 g of thionyl chloride (0.085 mol) and 40 mL of N,N-dimethylformamide were mixed and stirred until the reaction was completed, and the point The plate method judges the end of the reaction;

[0044] (2) adding water to the reaction system after the reaction in step (1) to quench and adjust the pH value to 10 with sodium hydroxide and extract with dichloromethane;

[0045] (3) Combine the organic phases, spin dry, add 20ml of acetone and heat until completely dissolved, cool to 10-20°C to crystallize, filter and dry to obtain light yellow solid powder.

[0046] After determination, the present embodiment prepares 3.6 g of light yellow solid powder with a purity of 96.5%. After mass spectrometry and nuclear magnetic detection, the result is 1 H-NMR (CDCl ...

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Abstract

The invention provides a preparation method of a ropivacaine hydrochloride impurity, and the preparation method of the ropivacaine hydrochloride impurity comprises the following steps: mixing 2, 6-dimethylaniline and a Vilsmeier-Haack reagent, reacting and purifying to obtain the ropivacaine hydrochloride impurity. The preparation method of the ropivacaine hydrochloride impurity is low in raw material cost and mild in reaction condition, the ropivacaine hydrochloride impurity can be generated through reaction only by mixing the reaction raw materials, conditions such as temperature control arenot needed, the preparation method is low in cost, no side reaction occurs, and the ropivacaine hydrochloride impurity prepared through the reaction is high in purity and yield.

Description

technical field [0001] The invention relates to the field of pharmaceutical impurities, in particular to a preparation method of ropivacaine hydrochloride impurities. Background technique [0002] Ropivacaine hydrochloride is an amide local anesthetic, a long-acting amide local anesthetic developed by Astra, Sweden, mainly used for surgical anesthesia and epidural anesthesia. Ropivacaine hydrochloride has dual effects of anesthesia and analgesia. Compared with amide local anesthetics such as bupivacaine, the drug has a longer drug action time and is less toxic to the heart. [0003] The impurities that may be produced during the production and storage of ropivacaine hydrochloride not only affect the purity of ropivacaine hydrochloride, but also affect the efficacy of the drug and may lead to toxic and side effects. Therefore, the research on the impurity of ropivacaine hydrochloride is of great significance. Publication No. CN105646482A discloses a method for preparing imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C257/12
CPCC07C257/12
Inventor 陈海龙柯海媚柳文俊李闫飞鞠云峰谭敏清
Owner GUANGDONG JIABO PHARM CO LTD
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