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Method for synthesizing N,N'-diisopropylcarbodiimide through oxidation of N,N'-diisopropylthiourea

A technology of diisopropylcarbodiimide and diisopropylthiourea, which is applied in the field of chemical synthesis, can solve the problems of high cost and low yield, and achieve low production cost, safe operation, and simple and easy-to-control process Effect

Inactive Publication Date: 2018-05-29
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the common synthetic methods have low yield and high cost. In view of the above limitations and shortcomings, the process needs to be improved.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 205kg of dichloromethane and 50kg of 40wt% dimethylamine aqueous solution to the reaction kettle, and dropwise add 420kg of sodium hypochlorite with 12% available chlorine below 15°C, separate and extract, dry with anhydrous magnesium sulfate to obtain the organic phase chlorodimethylamine Standby; add 60kg of N,N'-diisopropylthiourea and 20kg of caustic soda to the dry reaction kettle, add 380kg of chlorinated dimethylamine dropwise at a temperature below 30°C, and keep warm for 3 hours after the dropwise addition , after the heat preservation is completed, perform suction filtration, wash the filtrate with water, dry and distill off dichloromethane, and rectify to obtain N,N'-diisopropylcarbodiimide with a yield of 93.2%.

Embodiment 2

[0019] Add 210kg of dichloromethane and 50kg of 40wt% dimethylamine aqueous solution to the reaction kettle, and dropwise add 425kg of sodium hypochlorite with 12% available chlorine under the control of 15°C, separate and extract, dry with anhydrous sodium sulfate to obtain the organic phase chlorodimethylamine Standby; add 60kg of N,N'-diisopropylthiourea and 24kg of sodium carbonate to the dry reaction kettle, control the temperature below 30°C and dropwise add 376kg of chlorodimethylamine prepared in the previous step, and keep warm for 3 hours after the dropwise addition , after the heat preservation is completed, perform suction filtration, wash the filtrate with water, dry and distill dichloromethane, and then rectify to obtain N,N'-diisopropylcarbodiimide with a yield of 93.8%.

Embodiment 3

[0021] Add 200kg of dichloromethane and 50kg of 40wt% dimethylamine aqueous solution to the reaction kettle, add dropwise 430kg of sodium hypochlorite with 12% available chlorine below 15°C, separate and extract, dry with anhydrous calcium chloride to obtain the organic phase chlorodimethyl Amine for standby; add 60kg of N,N'-diisopropylthiourea, 22kg of sodium carbonate and caustic soda to the dry reaction kettle, control the temperature below 30°C and add 370kg of chlorinated dimethylamine dropwise prepared in the previous step, drop After the addition, keep it warm for 3 hours. After the heat preservation, carry out suction filtration, wash the filtrate with water, dry and distill off dichloromethane, and rectify to obtain N,N'-diisopropylcarbodiimide with a yield of 93.3%.

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PUM

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Abstract

The invention discloses a method for synthesizing N,N'-diisopropylcarbodiimide through oxidation of N,N'-diisopropylthiourea. Firstly, dimethylamine is oxidized with sodium hypochlorite, chloro-dimethylamine is obtained and used for oxidizing N,N'-diisopropylthiourea under the alkaline condition, and N,N'-diisopropylcarbodiimide is obtained. The yield reaches 93% or above, and meanwhile, the production cost is reduced due to recycling of chloro-dimethylamine.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for oxidatively synthesizing N,N'-diisopropylcarbodiimide from N,N'-diisopropylthiourea. Background technique [0002] N,N'-diisopropylcarbodiimide is a commonly used water loss agent. It is mainly used to activate carboxyl groups to promote the formation of amides and esters. The current common synthetic methods have low yields and high costs. In view of the above limitations and shortcomings, the process needs to be improved. Contents of the invention [0003] The object of the present invention is to provide a method for oxidatively synthesizing N,N'-diisopropylcarbodiimide with high product yield and low production cost from N,N'-diisopropylthiourea. [0004] The technical solution adopted by the present invention to solve the technical problem is: a method for oxidatively synthesizing N,N'-diisopropylcarbodiimide from N,N'-diisopropylthiourea, compr...

Claims

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Application Information

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IPC IPC(8): C07C267/00
CPCC07C267/00
Inventor 张路军张国辉韩超晨侯绪会王亮亮于西波
Owner SHANDONG HUIHAI PHARMA & CHEM