Synthesis method for 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate

A technology of dimethylaminopropyl and carbodiimide methyl, which is applied in the field of chemical intermediate preparation, can solve the problems such as literature reports on the method of carbodiimide methyl iodide, which is easy to industrialize and produce, Simple feeding and post-processing, good properties

Active Publication Date: 2014-03-26
ZHEJIANG BULK CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the prior art, there is no bibliographical report on the method of synthesizing 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide methyl iodide

Method used

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  • Synthesis method for 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate
  • Synthesis method for 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Add 4.3 kg of dichloromethane solvent into a reaction kettle, add 1.0 kg of 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide, start stirring, and pour in frozen brine, Start to cool down.

[0030] (2) When the temperature drops below 15°C, start to add 0.91 kg of methyl iodide dropwise. During the dropwise addition, control the temperature at 15°C to 25°C. After the dropwise addition of methyl iodide is completed, continue the reaction for 1 hour. During the reaction, the temperature Control at 15-25°C.

[0031] (3) After the reaction, add 2.15 kg of petroleum ether solvent, keep it warm for 2 hours, and control the temperature at 15-25°C.

[0032] (4) Put the material produced by the reaction in step (3) into a cloth bag, put it in a centrifuge and dry it at 60°C to obtain 1-ethyl-3-(3-dimethylaminopropyl)-carbodiethylene The finished product of ammonium iodide salt is 1.55 kg, and the yield is 81.2%. The finished product of 1-ethyl-3-(3-dimethylaminopropyl)-carbod...

Embodiment 2

[0034] (1) Add 4.3 kg of dichloromethane solvent into a reaction kettle, add 1.0 kg of 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide, start stirring, and pour in frozen brine, Start to cool down.

[0035] (2) When the temperature drops below 15°C, start to add 0.87 kg of methyl iodide dropwise. During the dropwise addition, control the temperature at 15°C to 25°C. After the dropwise addition of methyl iodide is completed, continue the reaction for 1 hour. During the reaction, the temperature Control at 15-25°C.

[0036] (3) After the reaction, add 2.15 kg of petroleum ether solvent, keep it warm for 2 hours, and control the temperature at 15-25°C.

[0037] (4) Put the material generated by the reaction in step (3) into a cloth bag, put it in a centrifuge and dry it to obtain 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide methyl iodide The finished product of salt is 1.45kg, and the yield is 75.92%. The finished product of 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide methy...

Embodiment 3

[0039] (1) Add 4.3 kg of dichloromethane solvent into a reaction kettle, add 1.0 kg of 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide, start stirring, and pour in frozen brine, Start to cool down.

[0040] (2) When the temperature drops below 15°C, start to add 0.90 kg of methyl iodide dropwise. During the dropwise addition, control the temperature at 15°C to 25°C. After the dropwise addition of methyl iodide is completed, continue to react for 1 hour. During the reaction, the temperature Control at 15-25°C.

[0041] (3) After the reaction, add 2.15 kg of petroleum ether solvent, keep it warm for 2 hours, and control the temperature at 15-25°C.

[0042] (4) Put the material generated by the reaction in step (3) into a cloth bag, put it in a centrifuge and dry it to obtain 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide methyl iodide The finished product of salt was 1.52kg, and the yield was 79.60%. The finished product of 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide methyl ...

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Abstract

The invention discloses a synthesis method for 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate. The synthesis method comprises the following steps of (1) adding 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine into a halohydrocarbon solvent, uniformly stirring the two materials, and cooling to be lower than 15 DEG C to obtain a solution A; (2) adding iodomethane into the solution A obtained in the step (1), controlling the temperature at lower than 25 DEG C for generating reaction, and obtaining a reaction solution B after the reaction is completely executed; (3) adding a hydrocarbon solvent into the reaction solution B obtained in the step (2) for crystallization, and collecting and drying crystallized solids to obtain the 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate. According to the synthesis method, the 1-ethyl-3-(3-dimethyl amino propyl)-carbonized diimine A iodate is obtained in a higher-yield way by selecting the proper solvent and controlling the temperature; the product is crystallized in a higher-purity way through the specific solvent; the synthesis method is convenient to operate and suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of preparation of chemical intermediates, in particular to a method for synthesizing 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide methyl iodide salt. Background technique [0002] In the past 20 years, carbodiimide series condensing agents, such as N,N-'dicyclohexylcarbodiimide (DCC), N,N-'diisopropylcarbodiimide (DIC), 1-ethane The research of base-(3-dimethylaminopropyl) carbodiimide hydrochloride (EDC.HCl) has aroused people's widespread interest, and because of its mild reaction conditions, high yield, good selectivity, and environmental protection It is widely used because of its friendliness and other characteristics. [0003] Wherein, 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride is 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide [structure such as The water-soluble salt formed by formula (I)] and hydrochloric acid is a dehydrating agent with high activity in the carbodiimide series. As the seco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C267/00
Inventor 李加尧陈江平傅桂萍
Owner ZHEJIANG BULK CHEM
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