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Process for preparing N,N'-dicyclohexyl carbodiimide by regeneration method

A dicyclohexylcarbodiimide, production process technology, applied in the field of N, can solve environmental problems such as pollution, waste of raw materials, etc., and achieve the effect of convenient operation, easy acquisition, and low cost

Inactive Publication Date: 2010-12-29
JINAN JUYE FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, DCC can also generate N, N'-dicyclohexyl urea (DCU) in the actual application process, if it is not recycled, it will cause waste of raw materials and environmental pollution

Method used

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  • Process for preparing N,N'-dicyclohexyl carbodiimide by regeneration method
  • Process for preparing N,N'-dicyclohexyl carbodiimide by regeneration method
  • Process for preparing N,N'-dicyclohexyl carbodiimide by regeneration method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 5.0kg of N, N'-dicyclohexylurea (DCU) raw materials into alkaline aqueous solution and soak three times to wash away the water-soluble impurities present in the raw materials. The soaked raw material was centrifugally dehydrated, put into a vacuum drying oven at 60° C., and dried to constant weight. The raw materials after constant weight are put into the polypropylene packing bag for standby.

[0026] Weigh 40.00 g of dried DCU, weigh 175.00 g of dichloromethane, add the two into a three-necked flask, weigh 35.50 g of phosphorus oxychloride, and add it to a 250 ml dropping funnel. Turn on the stirring device, then add phosphorus oxychloride dropwise to the reaction system, keep stirring for 2 hours after the addition, and keep the temperature between 40°C and 42°C during the reaction; pour the reaction solution into the dropping funnel, Then add 160g liquid industrial caustic soda (about 30%) in the there-necked flask, add 275ml distilled water. Turn on the stirr...

Embodiment 2

[0028] Weigh 40.00 g of dried DCU and 180.00 g of tetrahydrofuran, respectively add them into a three-necked flask, weigh 35.50 g of phosphorus oxychloride and add them into a 250 ml dropping funnel. Turn on the stirring device, then add phosphorus oxychloride dropwise to the reaction system, keep stirring for 2 hours after the addition, and keep the temperature between 40°C and 42°C during the reaction; pour the reaction solution into the dropping funnel, Then add 160g liquid industrial caustic soda (about 30%) in the there-necked flask, add 275ml distilled water. Turn on the stirring, add the reaction solution dropwise, continue stirring for 10 minutes after the addition, and keep the temperature below 40°C. Finally, the product was poured into a 1L separatory funnel, and the layers were allowed to stand. Release the lower organic phase, put it into a rotary evaporator to concentrate and crystallize to obtain the DCC product. The regeneration rate is 60%, and the DCC conte...

Embodiment 3

[0030] Weigh 40.00 g of dried DCU, weigh 150.00 g of acetonitrile, add the two into a three-necked flask, weigh 35.50 g of phosphorus oxychloride, and add it to a 250 ml dropping funnel. Turn on the stirring device, then add phosphorus oxychloride dropwise to the reaction system, keep stirring for 2 hours after the addition, and keep the temperature between 40°C and 42°C during the reaction; pour the reaction solution into the dropping funnel, Then add 130g industrial sodium carbonate in the there-necked flask, add 250ml distilled water. Turn on the stirring, add the reaction solution dropwise, continue stirring for 10 minutes after the addition, and keep the temperature below 40°C. Finally, the product was poured into a 1L separatory funnel, and the layers were allowed to stand. Release the lower organic phase, put it into a rotary evaporator to concentrate and crystallize to obtain the DCC product. The regeneration rate is 70%, and the DCC content of the product is 99.8%. ...

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Abstract

The invention discloses a process for preparing N,N'-dicyclohexyl carbodiimide by a regeneration method, which comprises the following steps of: removing impurities from N,N'-dicyclohexyl urea (DCU) serving as a raw material through alkaline wash, and performing regeneration by using an oxidizing agent; and reacting under stirring of an organic solvent at the temperature of between 40 and 42 DEG C for 0.15 to 2 hours to regenerate the N,N'-dicyclohexyl carbodiimide (DCC), wherein the regeneration rate is up to between 60 and 78 percent, and the DCC content of the product reaches over 99.5 percent. The process has the advantages of readily available raw materials, convenient operation and low cost, and provides the beneficial condition for the circular production and use of the DCC and particular the application to industry of medicine, the synthesis of amide and polypeptide and the like.

Description

technical field [0001] The invention relates to a production process of N,N'-dicyclohexylcarbodiimide, which belongs to the technical field of organic compound synthesis. Background technique [0002] N, N'-Dicyclohexylcarbodiimide, referred to as DCC, is a shrinking agent commonly used in organic synthesis and pharmaceutical manufacturing industries. It can dehydrate two molecules that cannot react originally to form a chemical bond. In my country, it is mainly used in the production of products such as amikacin and glutathione. [0003] The molecular formula of N,N'-dicyclohexylcarbodiimide is C 13 h 22 N 2 , the structural formula is: [0004] [0005] The preparation method of DCC can be divided into thiourea method and N, N'-dicyclohexyl urea (DCU) method. There are two synthetic methods in the thiourea method. Firstly, two molecules of cyclohexylamine and one molecule of carbon disulfide form corresponding thiourea derivatives, and then different reagents are u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C267/00
Inventor 高鑫张其坤
Owner JINAN JUYE FINE CHEM
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