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Preparation method of chloramphenicol impurity compound I

A compound, the technology of chloramphenicol, which is applied in the field of preparation of chloramphenicol impurities, can solve the problems of low yield and purity, long reaction time, cost of production enterprises, etc., achieve high yield and purity, save manpower and material resources, and react short time effect

Inactive Publication Date: 2021-06-22
WUHAN WUYAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the deficiencies in the prior art, the present invention provides a preparation method of chloramphenicol impurity compound I, which solves the problem that the existing preparation method of chloramphenicol impurity compound I is relatively complicated and needs to use a catalyst for catalytic reaction, the reaction time is long, and it is not easy Operation, yield and purity are low, production efficiency is low, and production companies need to spend high production costs

Method used

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  • Preparation method of chloramphenicol impurity compound I
  • Preparation method of chloramphenicol impurity compound I
  • Preparation method of chloramphenicol impurity compound I

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] S1. Add 10.0 g of refined L-amino, methyl trichloroacetate and 10.0 g of anhydrous methanol to the three-necked flask in sequence;

[0032] S2. After the feeding in step S1 is completed, stir and heat up, and raise the temperature inside the flask to 67°C;

[0033] S3. When the inner temperature of the flask reaches 67°C, the heat preservation reaction time is 1.25h;

[0034] S4, the heat preservation is finished, and the inner temperature of the flask is lowered to 25° C.;

[0035] S5, adding 20ml of methyl tert-butyl ether to the solution in step S4 for extraction, and then collecting the upper organic layer;

[0036] S6, adding 20ml of methyl tert-butyl ether to the lower aqueous layer for extraction, collecting the upper organic layer, and mixing with the organic layer collected in step S5, repeating the above operation, and extracting 3 times with methyl tert-butyl ether;

[0037] S7, adding anhydrous sodium sulfate to the mixed organic layer obtained in step S6 ...

Embodiment 2

[0043] S1. Add 10.0 g of refined L-amino and 9.20 g of methyl trichloroacetate to the three-necked flask in sequence

[0044] and anhydrous methanol 10.0g;

[0045] S2, after the addition of step S1 is completed, stir and heat up, and the temperature in the flask is raised to T;

[0046] S3, when the internal temperature of the flask reaches T, the heat preservation reaction time is 1.25h;

[0047] S4, the heat preservation is finished, and the inner temperature of the flask is lowered to 25° C.;

[0048] S5, adding 20ml of methyl tert-butyl ether to the solution in step S4 for extraction, and then collecting the upper organic layer;

[0049] S6, adding 20ml of methyl tert-butyl ether to the lower aqueous layer for extraction, collecting the upper organic layer, and mixing with the organic layer collected in step S5, repeating the above operation, and extracting 3 times with methyl tert-butyl ether;

[0050] S7, adding anhydrous sodium sulfate to the mixed organic layer obt...

Embodiment 3

[0056] S1. Add 10.0 g of refined L-amino and 9.20 g of methyl trichloroacetate to the three-necked flask in sequence

[0057] and anhydrous methanol 10.0g;

[0058] S2. After the feeding in step S1 is completed, stir and heat up, and raise the temperature inside the flask to 67°C;

[0059] S3. When the internal temperature of the flask reaches 67°C, the heat preservation reaction time is t;

[0060] S4, the heat preservation is finished, and the inner temperature of the flask is lowered to 25° C.;

[0061] S5, adding 20ml of methyl tert-butyl ether to the solution in step S4 for extraction, and then collecting the upper organic layer;

[0062] S6, adding 20ml of methyl tert-butyl ether to the lower aqueous layer for extraction, collecting the upper organic layer, and mixing with the organic layer collected in step S5, repeating the above operation, and extracting 3 times with methyl tert-butyl ether;

[0063] S7, adding anhydrous sodium sulfate to the mixed organic layer ob...

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Abstract

The invention discloses a preparation method of a chloramphenicol impurity compound I. The preparation method specifically comprises the following steps: S1, adding a refined L-amino compound, methyl trichloroacetate and absolute methanol into a reaction container, S2, stirring and heating, and raising the temperature in a flask, S3, after the temperature in the flask reaches 65-68 DEG C, carrying out a heat preservation reaction for 1 h or above, S4, cooling the temperature in the flask to room temperature, S5, adding methyl tert-butyl ether for extraction, and collecting an organic layer, S6, extracting again, and mixing the organic layers, S7, adding anhydrous sodium sulfate into the organic layer mixture, stirring and drying, and S8, spin-drying filtrate to obtain the target product. The preparation method of the chloramphenicol impurity compound I is simple in process, high in production efficiency, short in reaction time, easy to operate, high in yield and purity and high in production efficiency, does not need to use a catalyst for catalytic reaction, and does not need to spend high production cost on production enterprises.

Description

technical field [0001] The invention relates to the technical field of biochemical industry, in particular to a preparation method of chloramphenicol impurity. Background technique [0002] In the process of drug production, the research on intermediate impurities is an indispensable and very important part, and the residue of drug intermediate impurities will bring potential risks to the final drug products. The existence of these impurities not only affects the efficacy of the drug, but also causes problems in the production and storage process, and some impurities may even cause toxic and side effects. Therefore, analysis and research on drug impurities can not only ensure the safety, effectiveness and stability of drug use, but also provide a basis for quality assurance in the production and distribution process. Impurity standards refer to standard substances used for the identification, inspection and content determination of impurities. Therefore, in the process of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C231/24C07C233/18
CPCC07C231/02C07C231/24C07B2200/07
Inventor 赵涛涛任栋栋王成张伟肖应国张琦
Owner WUHAN WUYAO PHARMA
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