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Preparation method of dicyclohexylcarbodiimide

A technology of dicyclohexylcarbodiimide and dicyclohexylurea, which is applied in the field of organic compound synthesis, can solve environmental pollution and other problems, and achieve the effect of simple process

Inactive Publication Date: 2020-03-24
SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] DCU as a by-product of the reaction, direct discharge will cause environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 100g of dicyclohexyl urea to a mixed system consisting of 200mL of water and 200mL of methyl tert-butyl ether, stir and wash for 30min, filter it with suction, and dry it in a vacuum oven at 50°C until constant weight.

[0021] Put 50 g of dicyclohexyl urea and 300 mL of methyl tert-butyl ether into a dry three-necked flask, and stir evenly. At 25-35°C, add 42.5g of oxalyl chloride solution dropwise to the three-necked flask, control the dropping time to 3h, and the dropping temperature to , and keep warm for 0.5h after the dropping is completed. Take 26.8g of sodium hydroxide and make 15% lye. At 40-45°C, add the reaction solution dropwise to the alkaline solution, and control the dropping time to 6h. Then suction filtration, after the filtrate is layered, the organic phase is obtained, the solvent is removed by normal pressure distillation, and then vacuum distillation is carried out under the pressure of 1.35-1.54KPa, the fraction at 153-156°C is collected, and ...

Embodiment 2

[0023] Add 100g of dicyclohexyl urea into a mixed system consisting of 200mL of water and 200mL of dichloromethane and stir for 30min, filter it with suction and dry it in a vacuum oven at 50°C until it reaches a constant weight.

[0024] Put 50g of dicyclohexylurea and 400mL of dichloromethane into a dry three-necked flask, and stir evenly. At 10-20°C, add 31g of oxalyl chloride solution dropwise to the three-necked flask, control the dropping time to 4h, and the dropping temperature to , and keep warm for 0.5h after the dropping is completed. Take 20g of sodium hydroxide and make 15% lye. At 25-30°C, add the reaction solution dropwise to the alkali solution, and control the dropping time to 8h. Then suction filtration, the filtrate was distilled under normal pressure to remove the solvent, and then distilled under reduced pressure at a pressure of 1.35-1.54KPa to collect fractions at 153-156°C and vacuum-dried to obtain the product with a purity of 96.7% and a yield of 87.3...

Embodiment 3

[0026] Add 100g of dicyclohexyl urea into a mixed system consisting of 200mL of water and 200mL of methyl tetrahydrofuran, stir and wash for 30min, filter it with suction, and dry it in a vacuum oven at 50°C until constant weight.

[0027] Put 50 g of dicyclohexyl urea and 300 mL of methyl tetrahydrofuran into a dry three-necked flask, and stir evenly. At 25-35°C, add 31g of oxalyl chloride solution dropwise to the three-necked flask, control the dropping time to 1.5h, and the dropping temperature to , and keep warm for 0.5h after the dropping is completed. Take 20g of sodium hydroxide and make 15% lye. At 40-45°C, add the reaction solution dropwise to the alkaline solution, and control the dropping time to 4h. Then suction filtration, the filtrate was distilled under normal pressure to remove the solvent, and then distilled under reduced pressure at a pressure of 1.35-1.54KPa to collect fractions at 153-156°C and vacuum-dried to obtain the product with a purity of 95.2% and ...

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Abstract

The invention relates to a method for preparing dicyclohexylcarbodiimide by using recycled dicyclohexylurea, and the method comprises the following steps: adding the recycled dicyclohexylurea into a mixed system composed of water and an organic solvent, stirring, washing, filtering, and drying; uniformly stirring the dried dicyclohexylurea and an organic solvent, adding oxalyl chloride at a certain temperature for reaction, keeping the temperature for 0.5 h after dripping is finished, dripping reaction liquid into an aqueous solution of sodium hydroxide, filtering, standing filtrate for layering to obtain an organic phase, concentrating the organic phase, and performing reduced pressure distillation to obtain the dicyclohexylcarbodiimide. According to the method, DCU generated after DCC isused is regenerated into DCC, cyclic application is achieved, the technological method has the advantages of being safe, reliable and high in recovery rate, and industrial production can be achieved.

Description

technical field [0001] The invention discloses a preparation method of dicyclohexylcarbodiimide, which belongs to the technical field of organic compound synthesis. Background technique [0002] Dicyclohexylcarbodiimide (DCC), diisopropylcarbodiimide (DIC) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (EDCI) are currently commonly used three dehydrating condensing agents. When DCC is used as a dehydration condensation agent, it can be prepared after a short period of reaction at room temperature. The product after the reaction is dicyclohexyl urea (DCU). Since DCU has a small solubility in organic solvents, the reaction product is easy to separate and is widely used in Synthesis of polypeptides, nucleic acids, acids, anhydrides, aldehydes, ketones, etc. [0003] As a by-product of the reaction, direct discharge of DCU will cause environmental pollution. Converting DCU to DCC can not only reduce environmental pressure, but also recycle DCU and increase economic benefit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C267/00
CPCC07C267/00C07C2601/14
Inventor 王冠庆刘会邢长花魏蒙蒙
Owner SHANDONG JINCHENG KERUI CHEMICAL CO LTD
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