Method for synthesizing dicyclohexylcarbodiimide compound

A technology of dicyclohexylcarbodiimide and its synthesis method, which is applied in the direction of organic chemistry, can solve the problems of large safety hazards, high equipment requirements, inconvenient operation, etc., and achieve the goal of less three wastes, excellent product quality, and high total yield Effect

Inactive Publication Date: 2012-04-11
ZHEJIANG UNIV OF TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] However, this reaction requires high equipment, inconvenient

Method used

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  • Method for synthesizing dicyclohexylcarbodiimide compound
  • Method for synthesizing dicyclohexylcarbodiimide compound
  • Method for synthesizing dicyclohexylcarbodiimide compound

Examples

Experimental program
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Effect test

Embodiment 1

[0033] According to dicyclohexyl urea: the amount ratio of bis(trichloromethyl) carbonate feed material is 1: 1 feed intake, dicyclohexyl urea 112g (0.5mol), organic solvent is methyl tert-butyl ether 750mL, bis(trichloromethyl) Chloromethyl)carbonate 149g (0.5mol).

[0034] Dissolve bis(trichloromethyl)carbonate in 500mL of methyl tert-butyl ether, and slowly add it dropwise to a solution of dicyclohexylurea dissolved in 250mL of methyl tert-butyl ether at room temperature (20°C). After the addition, the temperature was raised to reflux temperature, and the reaction was completed after 5 hours of heat preservation reaction, and then the temperature was lowered to room temperature, and 100 mL of triethylamine was added dropwise to adjust the pH value of the reaction solution to 8. Tert-butyl ether was washed 3 times, filtered, and all filtrates (comprising the filtrate obtained by suction filtration and the filtrate obtained by filtering after washing) were combined and distil...

Embodiment 2

[0036] According to dicyclohexyl urea: bis (trichloromethyl) carbonate feed material ratio is 1: 0.5 feeding, dicyclohexyl urea 112g, bis (trichloromethyl) carbonate 74.5g, organic solvent is toluene 750mL.

[0037] The reaction temperature was 110° C., and other operations were the same as in Example 1 to obtain 95 grams of dicyclohexylcarbodiimide with a yield of 92% and a purity of 98%.

Embodiment 3

[0039] According to dicyclohexyl urea: bis (trichloromethyl) carbonate feed material ratio is 1: 0.33 feeding, dicyclohexyl urea 112g, organic solvent dichloromethane 500mL;

[0040] The reaction temperature was reflux temperature, and other operations were the same as in Example 1 to obtain 83.4 g of dicyclohexylcarbodiimide with a yield of 81% and a purity of 94%.

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Abstract

The invention discloses a synthetic method of a dicyclohexylcarbodiimide compound. The method comprises the following steps: taking dicyclohexylurea and di(trichloromethyl) carbonate as a raw material, fully reacting in an organic solvent A at the temperature of 20-110 DEG C, cooling to the room temperature after finishing the reaction, adding triethylamine and neutralizing to pH value of 7-8, post-treating a reaction solution to prepare the dicyclohexylcarbodiimide compound; wherein the organic solvent A is C1-C5 haloalkanes, C3-C8 fatty ester, ketones, ethers, benzene, toluene, xylene, chlorobenzene, nitrobenzene, cyclohexane or nitromethane. The method basically eliminates the problems of big hidden trouble of traditional technical safety and serious three wastes pollution. The method for synthesizing dicyclohexylcarbodiimide compound has the advantages of safety, reliability, simple process, less three wastes, small energy consumption, high overall yield, low cost and excellent product quality, and is suitable for industrialization production and has good economic benefit.

Description

(1) Technical field [0001] The invention relates to a synthesis method of a dicyclohexylcarbodiimide compound. (2) Background technology [0002] Dicyclohexylcarbodiimide (DCC) is a low-temperature dehydrating agent commonly used in industries and laboratories to synthesize aldehydes, ketones, amino acids, anhydrides, esters and other compounds. It is widely used in fine chemical industries such as medicine and pesticides. Since Sheeham first used DCC for peptide synthesis in 1955, DCC has become a well-known peptide condensation agent and one of the most important reagents for the acylation reaction of carboxylic acids and amines (or alcohols). The participation of DCC in the reaction has the characteristics of mild conditions, simple operation and high yield, and has extremely wide application in organic synthesis. [0003] Before the present invention is provided, the chemical synthesis method of dicyclohexylcarbodiimide in the prior art is more practical and mature meth...

Claims

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Application Information

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IPC IPC(8): C07C267/00
Inventor 苏为科李坚军蒲通翁意意王乃星戴佳佳
Owner ZHEJIANG UNIV OF TECH
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