Synthesis method of cyanoacetamide

A technology of cyanoacetamide and synthesis method, which is applied in chemical instruments and methods, dehydration preparation of carboxylic acid amides, preparation of organic compounds, etc., can solve problems such as potential safety hazards, long reaction time, and many side reactions, and achieve environmental protection High efficiency, high atom utilization, and the effect of improving product purity and yield

Active Publication Date: 2021-08-24
山东京博生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at problems such as low yield, long reaction time, many side reactions and potential safety hazards in existing synthetic methods, the present invention provides a cyanoethyl Synthetic method of amides to solve the above problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 102.1g (1.0mol) of malonamide and 204.2g of toluene in the mixing bottle and stir evenly. The temperature of the pipeline reactor is set to 50°C, the pressure is 0.5MPa, the flow rate of pump A is set to 1ml / min, and the flow rate of pump B is set to 1ml / min After reaching the set temperature, open the tail gas exhaust valve and triphosgene solution drip valve, open pump A to enter the toluene solution of malonamide, and open pump B to enter the toluene solution of triphosgene (297g triphosgene is dissolved in 891ml toluene), After 30 minutes, take a sample to detect the moisture content of the reaction liquid at the outlet of the reactor at 0.5%. After the sample injection, the reaction liquid in the receiving bottle is rectified at atmospheric pressure to recover toluene and a small amount of residual raw materials. Acetamide 84.0g, cyanoacetamide was detected by HPLC, the purity was calculated by external standard method: 98.5%, and the yield was 98.4%.

Embodiment 2

[0024] Weigh 112.3g (1.1mol) of malonamide and 377.1g of cyclohexane and stir them evenly in the mixing bottle. The temperature of the pipeline reactor is set to 80°C, the pressure is 1.5MPa, the flow rate of pump A is set to 2ml / min, and the flow rate of pump B is set to 2ml / min, after reaching the set temperature, open the tail gas evacuation valve and triphosgene solution drip valve, open the pump A to enter the cyclohexane solution of malonamide, and open the pump B to enter the cyclohexane solution of triphosgene (297g triphosgene solution in 891ml cyclohexane), after 30min, take a sample to detect the moisture content of the reaction solution at the outlet of the reactor is 0.2%. The temperature was 80°C, and then the temperature was lowered and centrifuged to obtain 93.2 g of cyanoacetamide. The cyanoacetamide was detected by HPLC, and the purity was calculated by the external standard method: 98.3%, and the yield was 99.0%.

Embodiment 3

[0026] Weigh 112.3g (1.1mol) of malonamide and 377.1g of cyclohexane and stir them evenly in the mixing bottle. The temperature of the pipeline reactor is set to 80°C, the pressure is 1.5MPa, the flow rate of pump A is set to 2ml / min, and the flow rate of pump B is set to 2ml / min, after reaching the set temperature, open the tail gas evacuation valve and triphosgene solution drip valve, open the pump A to enter the cyclohexane solution of malonamide, and open the pump B to enter the cyclohexane solution of triphosgene (297g triphosgene solution in 891ml cyclohexane), after 30min, take a sample to detect the moisture content of the reaction solution at the outlet of the reactor is 0.2%. The temperature was 80°C, and then the temperature was lowered and centrifuged to obtain 93.2 g of cyanoacetamide. The cyanoacetamide was detected by HPLC, and the purity was calculated by the external standard method: 98.3%, and the yield was 99.0%.

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Abstract

The invention relates to a synthesis method of cyanoacetamide, and belongs to the technical field of organic synthesis. According to the method, a tubular reactor is used as reaction equipment, malonamide is used as a raw material, and cyanoacetamide is generated under the action of triphosgene. The triphosgene with relatively high reaction activity is used, so that the activation energy of the reaction can be reduced, and the forward proceeding of the reaction is promoted; a pipeline reactor is used as reaction equipment, so that the mass and heat transfer effect of a reaction system can be improved, the reaction time and the retention time of a product in the reaction system are further shortened, and the product purity and yield are effectively improved. The atom utilization rate is high, the by-product ammonium chloride can be sold as a product or used for other reactions, and the recovered solvent and the treated rectification base solution can be used for reactions; and only a small amount of activated carbon waste residues are generated, so that the environment-friendly benefit is high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis method of cyanoacetamide. Background technique [0002] Cyanoacetamide is an important intermediate for the synthesis of pesticides and medicines, and can be used to prepare flonicamid, malononitrile, milrinone, opprinone, etc. Currently, the main methods for synthesizing cyanoacetamide are the following two: (1) Reaction of methyl cyanoacetate with methanol solution of ammonia; (2) Hydrolysis of malononitrile to obtain cyanoacetamide. Wherein method (1) reaction time is long, and reaction exothermic heat is big, is difficult for temperature control, and finished product yield is low. There are potential safety hazards in the industrial production process, and there is methanol in the reaction system, which is flammable and explosive, and has great potential safety hazards. Adopt malononitrile and water in the method (2), the reaction activity ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/00C07C253/20C07C253/34C07C255/19B01J19/24
CPCC07C253/00C07C253/20C07C253/34B01J19/2415C07C255/19
Inventor 景伟伟张永军于连友王光金张思思侯继敏李冰洁
Owner 山东京博生物科技有限公司
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