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Method for synthesizing 2-azetidinone

A technology of azetidinone and solution, which is applied in the field of synthesizing 2-azetidinone, can solve the problems of difficult control of precision, low purity of 2-azetidinone, numerous uncontrollable factors, etc. The effect of high precision of finished product, controllable temperature and reaction time

Inactive Publication Date: 2018-06-01
ZHONGSHAN DEGAOXING INTPROP CENT LLP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The existing synthetic method of 2-azetidinone is to react fluorobenzoyl butyric acid with pivaloyl chloride, and use a chiral auxiliary to acylate the product to obtain a ketone; then reduce the ketone in the presence of a chiral auxiliary Alcohol; react chiral alcohol, imine and silyl protecting agent, and then condense the protected compound to obtain β-amide, but the purity of 2-azetidinone synthesized by this method is low, and it is uncontrollable during the synthesis process There are many factors, and its accuracy is not easy to control

Method used

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  • Method for synthesizing 2-azetidinone

Examples

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Effect test

Embodiment 1

[0020] A method for synthesizing 2-azetidinone, the specific steps of the method are as follows:

[0021] S1: Add 10g of D-methyl lactate and 15g of bromochloromethane into the reaction flask, add 20ml of 4-dimethylaminopyridine solution, stir for 30min, and mix them uniformly to form a mixed solution;

[0022] S2: Cool the mixed solution to 0°, then slowly add the triethyl phosphite solution dropwise, after the addition is completed, remove the cooling device, raise the temperature to room temperature and react for 4 hours, after the reaction is complete, dilute the reaction solution with 100ml of pure water;

[0023] S3: The reaction solution was extracted with 60 ml of ether solution, dried over anhydrous sodium sulfate, and the solvent was removed to obtain an intermediate product;

[0024] S4: Add 5g of sodium hydroxide solution to the intermediate product, and heat the reaction, the temperature of the heating reaction is 50°C, and the reaction time is 1h;

[0025] S5: A...

Embodiment 2

[0030] A method for synthesizing 2-azetidinone, the specific steps of the method are as follows:

[0031] S1: Add 15g of D-methyl lactate and 20g of bromochloromethane into the reaction flask, add 25ml of 4-dimethylaminopyridine solution, stir for 30min, and mix them uniformly to form a mixed solution;

[0032] S2: Cool the mixed solution to 3°, then slowly add the triethyl phosphite solution dropwise, after the addition is completed, remove the cooling device, raise the temperature to room temperature and react for 5 hours, after the reaction is complete, dilute the reaction solution with 200ml of pure water;

[0033] S3: The reaction solution was extracted with 80 ml of diethyl ether solution, dried over anhydrous sodium sulfate, and the solvent was removed to obtain an intermediate product;

[0034] S4: Add 10 g of sodium hydroxide solution to the intermediate product, and heat the reaction. The temperature of the heating reaction is 60° C., and the reaction time is 1.5 h; ...

Embodiment 3

[0040] A method for synthesizing 2-azetidinone, the specific steps of the method are as follows:

[0041] S1: Add 13g of methyl D-lactate and 18g of bromochloromethane into the reaction flask, add 23ml of 4-dimethylaminopyridine solution, stir for 40min, and mix them uniformly to form a mixed solution;

[0042] S2: Cool the mixed solution to 2°, then slowly add the triethyl phosphite solution dropwise, after the addition is completed, remove the cooling device, raise the temperature to room temperature and react for 5 hours, after the reaction is complete, dilute the reaction solution with 150ml of pure water;

[0043] S3: The reaction solution was extracted with 70 ml of ether solution, dried over anhydrous sodium sulfate, and the solvent was removed to obtain an intermediate product;

[0044] S4: Add 7g of sodium hydroxide solution to the intermediate product, and heat the reaction, the temperature of the heating reaction is 55°C, and the reaction time is 1.5h;

[0045] S5:...

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Abstract

The invention discloses a method for synthesizing 2-azetidinone in the technical field of chemical synthesis. The method comprises specific steps as follows: S1, preparation of a mixed solution; S2, addition of an aid and dilution; S3, solution extraction and drying; S4, addition of sodium hydroxide and heating; S5, solution neutralization, water washing and drying; S6, toluene dissolution; S7, detection with a chromatograph; S8, product purification treatment. The synthesis method is simple, the prepared finished product has high accuracy, the temperature and the reaction time are controllable in the synthesis process, no raw material waste phenomenon is caused in the synthesis process and the method is suitable for large-scale production in a factory.

Description

technical field [0001] The invention discloses a method for synthesizing 2-azetidinone, and specifically belongs to the technical field of chemical synthesis. Background technique [0002] The existing synthetic method of 2-azetidinone is to react fluorobenzoyl butyric acid with pivaloyl chloride, and use a chiral auxiliary to acylate the product to obtain a ketone; then reduce the ketone in the presence of a chiral auxiliary Alcohol; react chiral alcohol, imine and silyl protecting agent, and then condense the protected compound to obtain β-amide, but the purity of 2-azetidinone synthesized by this method is low, and it is uncontrollable during the synthesis process There are many factors, and its accuracy is not easy to control. For this reason, we proposed a method for synthesizing 2-azetidinone and put it into use to solve the above problems. Contents of the invention [0003] The purpose of the present invention is to provide a method for synthesizing 2-azetidinone ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D205/08
CPCC07D205/08
Inventor 谢小坚梁荣强
Owner ZHONGSHAN DEGAOXING INTPROP CENT LLP
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