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Preparation method of 1-ethyl-(3-dimethyl amino propyl) carbodiimide hydrochloride

A technology of dimethylaminopropyl and carbodiimide hydrochloride, which is applied in the direction of organic chemistry, can solve the problems of cumbersome steps, complicated operation, and unsuitability for industrial production, and achieve simplified operation steps, high purity, and easy The effect of implementation

Inactive Publication Date: 2019-02-22
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has cumbersome steps, complex operation, and uses a large amount of organic solvents, which is not suitable for industrial production

Method used

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  • Preparation method of 1-ethyl-(3-dimethyl amino propyl) carbodiimide hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0036] Add 195g of carbon disulfide and 198g of 40% mass concentration liquid caustic soda into a 2000ml reaction bottle, slowly add 143g of ethylamine dropwise, keep the temperature at 25°C, add dropwise for 60min, stir and keep warm for 90min, and react to generate EDTC; Dissolve 172g of the ester in 240g of cyclohexane, slowly drop it into the EDTC reaction solution, keep the temperature at 20°C, add the mixture for 90 minutes, and keep it warm for 150 minutes.

[0037] Transfer the material to an oil bath for distillation. Distill at an oil bath temperature of about 120°C until nothing comes out. Take the fraction and separate it in a separatory funnel. The upper layer of oil is EITC. 197g of the product is obtained with a yield of 89% and a purity of >99% %.

[0038] Add 600g of water to a 2000ml reaction bottle, add 273g of N,N-dimethyl-1,3-propanediamine, slowly add 197g of EITC dropwise, keep the temperature at 18°C, complete the dropwise addition in 60min, keep warm f...

Embodiment 3

[0041] Add 200g of carbon disulfide and 240g of 40% mass concentration liquid caustic soda into a 2000ml reaction bottle, slowly drop into 167g of ethylamine, keep the temperature at 15°C, add the time for 30min, stir and keep warm for 90min, and react to generate EDTC; Dissolve 149g of ester in 280g of petroleum ether, slowly drop into the EDTC reaction solution, keep the temperature at 27°C, add for 90min, and keep warm for 120min.

[0042] Transfer the material to an oil bath for distillation. Distill at an oil bath temperature of about 130°C until nothing comes out. Take the fraction and separate it in a separatory funnel. The upper layer of oil is EITC. 200g of the product is obtained with a yield of 90% and a purity of >99% %.

[0043] Add 600g of water to a 2000ml reaction bottle, add 300g of N,N-dimethyl-1,3-propanediamine, slowly add 200g of EITC dropwise, keep the temperature at 26°C, complete the dropwise addition in 30 minutes, and keep it warm for 120 minutes to o...

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PUM

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Abstract

The invention relates to a preparation method of 1-ethyl-(3-dimethyl amino propyl) carbodiimide hydrochloride and belongs to the technical field of medicine intermediates. The preparation method comprises the following seven steps: carrying out a reaction to generate EDTC; preparing an EITC coarse product; carrying out distillation and fractionation; preparing an intermediate; preparing EDC; and preparing a target product. The preparation method provided by the invention has the characteristics of being high in product yield and purity, simple in operating step, easy to implement and suitablefor industrial production.

Description

technical field [0001] The invention relates to a preparation method of 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride, belonging to the technical field of pharmaceutical intermediates. Background technique [0002] 1-Ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride, referred to as EDC hydrochloride, with molecular formula C8H17N3·HCl, is a water-soluble peptide coupling agent and a general carbonyl activating reagent. It can be used for bonding between amides and secondary amines, reacting with phosphate groups, cross-linking proteins and nucleic acids, preparing immune cross-links, and carbonyl modification in proteins, etc. [0003] In 1996, Japanese patent JPH08198836A used ethylamine as raw material to prepare ethyl isothiocyanate, then reacted with N,N-dimethyl-1,3-propanediamine, and then used sodium hypochlorite oxidative desulfurization to obtain the product with a yield of 32%. However, the yield of this method is low, and it is not suitable f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C267/00
CPCC07C267/00C07C331/20C07C333/20C07C335/08
Inventor 崔宝龙李凯宋君韩扬司维森
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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