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A kind of preparation method of ethyl 7-chloro-2-oxoheptanoate

A technology for ethyl oxoheptanoate and anhydrous ethyl ether, which is applied in the preparation field of synthesizing ethyl 7-chloro-2-oxoheptanoate by means of a grignard method, can solve problems such as difficulty in preparing Grignard reagents, and reduce production cost, quality improvement

Active Publication Date: 2015-09-02
河北慧林生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far, it is difficult to prepare Grignard reagents in benzene solvents, especially toluene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The first step is the preparation of the Grignard reaction solution

[0044]5 kilograms of magnesium metal and 140 kilograms of anhydrous ether are added to dryness and stirred in a nitrogen-protected reactor; 100 kilograms of 1-bromo-5-chloropentane and 176 kilograms of anhydrous toluene are mixed and added to In the dropping funnel, slowly drop it into the above reaction kettle; after the initiation reaction is successful, lower the temperature and continue the dropwise reaction, and add 8.2 kg of metal magnesium strips into it three times at the same time, the reaction temperature is controlled at -15 ° C, and the metal magnesium It should be added completely 30 minutes before the mixed liquid is added to ensure sufficient reaction time; after the reaction is completed, the Grignard reaction liquid is obtained, and it is sealed and frozen for future use;

[0045] The second step condensation reaction

[0046] Add 80 kg of diethyl oxalate and 176 kg of anhydro...

Embodiment 2

[0050] The first step is the preparation of the Grignard reaction solution

[0051] 5 kilograms of magnesium metal and 145 kilograms of anhydrous ether are added to dryness and stirred in a nitrogen-protected reactor; 100 kilograms of 1-bromo-5-chloropentane and 180 kilograms of anhydrous toluene are mixed and added to In the dropping funnel, slowly drop into the above-mentioned reaction kettle; after the initiation reaction is successful, lower the temperature and continue the dropwise reaction, and add 8.1 kg of metal magnesium strips into it in four times at the same time, the reaction temperature is controlled at 0 ° C, and the metal magnesium It should be added completely 40 minutes before the mixed liquid is added to ensure sufficient reaction time; after the reaction is completed, the Grignard reaction liquid is obtained, and it is sealed and frozen for future use;

[0052] The second step condensation reaction

[0053] Add 80 kg of diethyl oxalate and 180 kg ...

Embodiment 3

[0057] The first step is the preparation of the Grignard reaction solution

[0058] 5 kilograms of magnesium metal and 130 kilograms of anhydrous ether are added to dryness and stirred in a nitrogen-protected reactor; 100 kilograms of 1-bromo-5-chloropentane and 165 kilograms of anhydrous toluene are mixed and added to In the dropping funnel, slowly drop it into the above reaction kettle; after the initiation reaction is successful, lower the temperature and continue the dropwise reaction, and add 8.0 kg of metal magnesium strips to it in five times at the same time, the reaction temperature is controlled at -10 ° C, and the metal Magnesium should be added completely 45 minutes before the mixed liquid is added to ensure sufficient reaction time; after the reaction is completed, the Grignard reaction liquid is obtained, which is sealed and frozen for future use;

[0059] The second step condensation reaction

[0060] Add 80 kg of diethyl oxalate and 165 kg of anhydrou...

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Abstract

The invention belongs to the technical field of preparation of pharmaceutical intermediates and discloses a preparation method of ethyl 7-chloro-2-oxoheptanoate. The preparation method comprises the preparation steps of performing Grignard reaction on 1-bromo-5-chloropentane and magnesium to obtain a Grignard reagent reaction solution; performing condensation reaction on the reaction solution and diethyl oxalate, and performing treatment to obtain a crude product of ethyl 7-chloro-2-oxoheptanoate; performing condensation reaction and hydrolysis reaction on the crude product and a purifying agent of a hydrazine compound, and rectifying to obtain ethyl 7-chloro-2-oxoheptanoate. The method for preparing ethyl 7-chloro-2-oxoheptanoate has the characteristics of relatively high product yield, low production cost and little pollution in preparation process.

Description

technical field [0001] The invention belongs to the technical field of preparation of pharmaceutical intermediates, in particular to a preparation method for synthesizing ethyl 7-chloro-2-oxoheptanoate by a Grignard method. Background technique [0002] Cilsatatin (cilsatatin), the chemical name is (+)-(Z)-7-[(2R)-(2-amino-2-carboxyethyl)sulfur]-2-[(1S)-(2, 2-Dimethylcyclopropanecarboxamido)-2-heptenoic acid is a renal dehydrodipeptidase inhibitor developed by Merck in the United States, which can inhibit the broad-spectrum antimicrobial drug imine currently in clinical use. The renal metabolism of imipenem can increase the blood inhibitory concentration of imipenem while reducing renal toxicity, and the curative effect is very significant. Therefore, the compound preparation of cilastatin and imipenem can be used as a broad-spectrum antibacterial Drugs are increasingly used clinically. [0003] Imipenem is a thiamycin antibacterial drug with a carbapenem ring. Its antib...

Claims

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Application Information

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IPC IPC(8): C07C69/716C07C67/60C07C67/343
CPCC07C67/343C07C67/60C07C69/716
Inventor 孙德春
Owner 河北慧林生物科技有限公司
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