Production technique of N,N'-dicyclo hexylcar bodiimide

A dicyclohexylcarbodiimide, production process technology, applied in the field of polypeptide dehydration condensation agent N, can solve difficult desulfurization and other problems, achieve the effect of reducing production cost and improving product quality

Active Publication Date: 2008-01-02
SHANDONG JINCHENG PHARMACEUTICAL GROUP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] It is difficult to completely desulfurize by traditional process

Method used

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  • Production technique of N,N'-dicyclo hexylcar bodiimide
  • Production technique of N,N'-dicyclo hexylcar bodiimide
  • Production technique of N,N'-dicyclo hexylcar bodiimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 30g of cyclohexylamine to 200ml of xylene, stir and add 10g of carbon disulfide dropwise, control the temperature at 50°C, reflux for 3 hours, heat filter, filter out the alkali sulfide, cool down the crystal and suction filter, dry to obtain white crystal N,N-di Cyclohexylurea, yield 98%.

[0033] Add 30 g of N, N-dicyclohexylurea to 300 ml of benzene, add 1 g of catalyst (TEBA), stir and heat, add dropwise 100 ml of sodium hypochlorite solution (concentration 30%) at 70 ° C, stir for 2 hours, extract with water, and then use the same The sodium hypochlorite and catalyzer carry out secondary oxidation, and step is the same as above.

[0034] Add 20 g of the by-product sodium sulfide in the first step to the extract, under alkaline conditions, control the pH value to 9, stir and react for 2 hours, filter and extract with water separation, remove sulfur, and carry out distillation and rectification of the organic phase to obtain the product. The yield is 92%, and th...

Embodiment 2

[0036] Add 80 kg of cyclohexylamine to 400 kg of xylene, stir and add 40 kg of carbon disulfide dropwise, control the reaction temperature at 60° C., reflux for 3 hours, heat filter, filter out alkali sulfide (for standby), cool down the crystal and suction filter, and dry to obtain white crystal N. N-Dicyclohexylurea.

[0037] Add N,N-dicyclohexyl urea 700kg in 500kg benzene. Add 30 kg of catalyst polyethylene glycol, stir and heat, add dropwise 800 kg of sodium hypochlorite solution (concentration 30%) at 70 ° C, stir for 2 hours, and extract with water. Then use 800 kg of sodium hypochlorite solution (concentration 30%) and 3 kg of polyethylene glycol Secondary oxidation, the steps are the same as above.

[0038] Add 200 kg of the by-product sodium sulfide in the first step into the extract (organic phase), under alkaline conditions, control the pH value to 8, stir and react for 2 hours, filter and extract with water separation, remove sulfur, and carry out distillation an...

Embodiment 3

[0040] With embodiment 1, difference is that the consumption of catalyst TEBA is 1.5kg. The product yield is 93%, and the product purity is above 99.5%.

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Abstract

The invention discloses a production technology of N, N'-dicyclo hexylcar bodiimide, which comprises the following steps: generating dicyclohexyl sulfourea and sodium sulfide with cyclohexylamine and carbon bisulphide; generating N, N'-dicyclo hexylcar bodiimide by oxygenizing dicyclohexyl sulfourea twice with sodium hypochlorite and removing hydrogen sulfide. The invention is characterized by the following: adding the accelerant when dicyclohexyl sulfourea is oxygenized by sodium hypochlorite; applying triethyl benzyl ammonium chloride(TEBA)or carbowax as the accelerant; adding sodium sulfide which is generated in the first step reaction in order to removing sulfur by reacting with sulfur in the organic phase after oxygenizing twice. The invention guarantees the sufficient oxidation reaction, which reduces the production cost, and improves the product quality.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and is an improvement on the production process of polypeptide dehydration condensation agent N, N'-dicyclohexylcarbodiimide. Background technique [0002] N, N'-Dicyclohexylcarbodiimide, referred to as DCC, the molecular formula is: C 13 h 22 N 2 , the structural formula is: [0003] [0004] Relative molecular mass: 206.33, white to pale yellow crystalline solid or transparent liquid, melting point 33-35°C, boiling point 154-156°C (1.47KPa). Insoluble in water, soluble in benzene, ethanol, ether. N,N'-Dicyclohexylcarbodiimide is mostly used in the synthesis of peptide drugs as a dehydration condensation agent, and the product purity is very high, which is difficult to meet by traditional techniques. [0005] The traditional production process of N,N'-dicyclohexylcarbodiimide is roughly as follows: [0006] The reaction of cyclohexylamine and carbon disulfide generates dicyclohexyl...

Claims

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Application Information

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IPC IPC(8): C07C251/02C07C249/02
Inventor 张学波郑庚修刘承平候乐伟解春章
Owner SHANDONG JINCHENG PHARMACEUTICAL GROUP CO LTD
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