Synthesis and process of N, N-diisopropylaminoacetonitrile

Abstract

The invention discloses a synthesis and process of N, N-diisopropylaminoacetonitrile, and belongs to the technical field of organic synthetic chemistry, the N, N-diisopropylaminoacetonitrile comprises the following synthesis raw materials: diisopropylamine, formaldehyde, sodium cyanide, hydrochloric acid and water, the feeding molar ratio of diisopropylamine to formaldehyde to sodium cyanide is 1: 1.1: 1; the method comprises the following steps: S1, preparing equipment required for synthesis: two 50L reaction kettles, one 100L reaction kettle, one 3m < 2 > condenser, one 1L glass water segregator, one cold and hot all-in-one machine, one water circulation vacuum pump and one 5L receiving bottle; s2, equipment inspection: all appliances are used after being washed with 3% sodium hypochlorite; s3, 5 kg of sodium cyanide is put into a 50 L reaction kettle, 30 kg of water is pumped into the reaction kettle in a vacuum mode, stirring and dissolving are conducted, and the sodium cyanide aqueous solution is obtained.According to the method, expensive chloroacetonitrile reaction is avoided, the production cost is greatly reduced, operation is easy and convenient, a complex refining process is not needed, the production and refining difficulty of the product is effectively reduced, and the environment-friendly requirement is met; and the method can be widely applied to production.

Description

Technical Field

[0001] This invention belongs to the field of organic synthesis chemistry technology, and particularly relates to the synthesis and process of N,N-diisopropylaminoacetonitrile. Background Technology

[0002] Currently, the synthesis of N,N-diisopropylaminoacetonitrile mainly involves the catalytic reaction of diisopropylamine and chloroacetonitrile in an inorganic base and solvent, followed by extraction and distillation purification to obtain the product. However, this process has significant drawbacks: firstly, the raw material chloroacetonitrile is expensive, significantly increasing production costs; secondly, it involves numerous side reactions, resulting in low yields, high levels of impurities, and difficulty in purification, thus limiting its large-scale production application. Therefore, developing a new, low-cost, and easy-to-operate synthetic process is urgently needed. Summary of the Invention

[0003] To address the problems of existing technologies, this invention provides a synthesis and process for N,N-diisopropylaminoacetonitrile, which avoids the use of expensive chloroacetonitrile, significantly reducing production costs. The process is simple to operate, requires no complex purification process, effectively reduces the difficulty of production and purification, meets environmental protection requirements, and facilitates its widespread application in production. This invention solves the problem that the current synthesis of N,N-diisopropylaminoacetonitrile mainly involves the catalytic reaction of diisopropylamine and chloroacetonitrile in inorganic alkali and solvents, followed by extraction and distillation purification. However, this process has significant drawbacks: firstly, the raw material chloroacetonitrile is expensive, greatly increasing production costs; secondly, it involves numerous side reactions, resulting in low yields, high impurities, and difficulty in purification, thus limiting its large-scale production application.

[0004] The present invention is achieved by synthesizing N,N-diisopropylaminoacetonitrile, comprising the following raw materials: diisopropylamine, formaldehyde, sodium cyanide, hydrochloric acid and water, wherein the molar ratio of diisopropylamine, formaldehyde and sodium cyanide is 1:1.1:1.

[0005] A process for synthesizing N,N-diisopropylaminoacetonitrile, applicable to the synthesis of the aforementioned N,N-diisopropylaminoacetonitrile, includes the following steps:

[0006] S1. Equipment required for synthesis: 2 x 50L reactors, 1 x 100L reactor, 1 x 3㎡ condenser, 1 x 1L glass water separator, 1 x integrated heating and cooling unit, 1 x water circulation vacuum pump, and 1 x 5L receiving bottle.

[0007] S2. Check the equipment: Check the sealing condition to ensure normal use, wear appropriate personal protective equipment, and rinse all tools with 3% sodium hypochlorite before use;

[0008] S3. Preparation of sodium cyanide aqueous solution: Add 5 kg of sodium cyanide to a 50 L reactor, vacuum pump in 30 kg of water, stir to dissolve and obtain sodium cyanide aqueous solution for later use.

[0009] S4. Main reaction stage: First, vacuum pump 25.82 kg of 40% diisopropylamine and 8.27 kg of 37% formaldehyde into a 100L reactor. Cool to 10℃, add 2 kg of hydrochloric acid to the dropping funnel, and add it dropwise into the 100L reactor. Adjust the pH to 10 and finish the addition after 2 hours. Then, add the prepared sodium cyanide aqueous solution dropwise and finish the addition after 2 hours. Keep the temperature at 20℃ for 2 hours, let it stand for about 30 minutes, separate the lower water layer, let the water layer stand and transfer it to the wastewater treatment vessel. After washing with sodium hypochlorite and testing with cyanide test paper, transfer it to the sewage treatment plant after it passes the test.

[0010] S5. Post-processing of the product: The upper organic phase is transferred to the dehydration kettle. The temperature is raised to 80°C to start the separation of water. The organic layer is condensed by the condenser and then flows back to the reaction kettle through the water separator. The water layer is condensed by the condenser and then flows to the lower layer of the water separator to the receiving bottle. It is then transferred to the sodium cyanide preparation kettle. The process ends when the temperature rises to 120°C. The material is then discharged and packed into barrels.

[0011] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0012] Cost reduction: Replacing expensive chloroacetonitrile with inexpensive formaldehyde and sodium cyanide systems significantly reduces raw material costs and improves production economics;

[0013] Simplified process: After the reaction is completed, the water layer is separated by standing. The upper organic layer is refluxed to remove water to obtain the product. The operation is simpler and more convenient. The lower water layer is washed with sodium hypochlorite and then safely discharged after being tested with sodium cyanide test paper. The post-treatment only requires standing to separate water and reflux to remove water. The operation is simple and does not require a complicated purification process, which reduces the difficulty of production and purification and is conducive to large-scale industrial production.

[0014] Environmental safety: The water layer is properly treated (washed with sodium hypochlorite and discharged after passing the test), effectively controlling the risk of cyanide pollution and meeting environmental protection requirements.

[0015] This invention avoids the use of expensive chloroacetonitrile reaction, greatly reducing production costs. It is easy to operate, requires no complicated refining process, effectively reduces the difficulty of production and refining of the product, meets environmental protection requirements, and is conducive to its widespread application in production. Attached Figure Description

[0016] Figure 1 This is a synthesis reaction process diagram provided in the embodiments of the present invention. Detailed Implementation

[0017] To further understand the invention's content, features, and effects, the following embodiments are provided, and detailed descriptions are given in conjunction with the accompanying drawings.

[0018] The structure of the present invention will now be described in detail with reference to the accompanying drawings.

[0019] refer to Figure 1 As shown in the embodiment of the present invention, an N,N-diisopropylaminoacetonitrile synthesis method is provided, comprising the following raw materials: diisopropylamine, formaldehyde, sodium cyanide, hydrochloric acid and water, wherein the molar ratio of diisopropylamine, formaldehyde and sodium cyanide is 1:1.1:1.

[0020] A process for synthesizing N,N-diisopropylaminoacetonitrile, applicable to the synthesis of the aforementioned N,N-diisopropylaminoacetonitrile, includes the following steps:

[0021] S1. Equipment required for synthesis: 2 x 50L reactors, 1 x 100L reactor, 1 x 3㎡ condenser, 1 x 1L glass water separator, 1 x integrated heating and cooling unit, 1 x water circulation vacuum pump, and 1 x 5L receiving bottle.

[0022] S2. Check the equipment: Check the sealing condition to ensure normal use, wear appropriate personal protective equipment, and rinse all tools with 3% sodium hypochlorite before use;

[0023] S3. Preparation of sodium cyanide aqueous solution: Add 5 kg of sodium cyanide to a 50 L reactor, vacuum pump in 30 kg of water, stir to dissolve and obtain sodium cyanide aqueous solution for later use.

[0024] S4. Main reaction stage: First, vacuum pump 25.82 kg of 40% diisopropylamine and 8.27 kg of 37% formaldehyde into a 100L reactor. Cool to 10℃, add 2 kg of hydrochloric acid to the dropping funnel, and add it dropwise into the 100L reactor. Adjust the pH to 10 and finish the addition after 2 hours. Then, add the prepared sodium cyanide aqueous solution dropwise and finish the addition after 2 hours. Keep the temperature at 20℃ for 2 hours, let it stand for about 30 minutes, separate the lower water layer, let the water layer stand and transfer it to the wastewater treatment vessel. After washing with sodium hypochlorite and testing with cyanide test paper, transfer it to the sewage treatment plant after it passes the test.

[0025] S5. Post-processing of the product: The upper organic phase is transferred to the dehydration kettle. The temperature is raised to 80°C to start the separation of water. The organic layer is condensed by the condenser and then flows back to the reaction kettle through the water separator. The water layer is condensed by the condenser and then flows to the lower layer of the water separator to the receiving bottle. It is then transferred to the sodium cyanide preparation kettle. The process ends when the temperature rises to 120°C. The material is then discharged and packed into barrels.

[0026] Working principle of the invention:

[0027] In operation, the process begins with step S2 to ensure equipment cleanliness and safety, preventing impurities from interfering with the reaction or posing safety risks. In step S3, when preparing the sodium cyanide aqueous solution, water acts as a solvent, causing sodium cyanide to dissociate into cyanide ions, providing active species for the subsequent nucleophilic reaction. The main reaction stage, S4, is the core process. 40% diisopropylamine and 37% formaldehyde are first mixed at 10°C. At this point, the amino group in diisopropylamine acts as a nucleophile, attacking the carbonyl group of formaldehyde to undergo nucleophilic addition, forming an imine intermediate. Hydrochloric acid is added to adjust the pH to 10, ensuring the nucleophilic activity of the amino group while preventing excessive acidity that could lead to protonation and deactivation of the amine. Subsequently, the added sodium cyanide aqueous solution further reacts with the imine intermediate as a nucleophile. The precursor for N,N-diisopropylaminoacetonitrile is generated. Holding the mixture at 20°C for 2 hours promotes complete reaction and ensures the intermediate is fully converted into the target product. After standing, the organic phase (containing the target product) and the aqueous phase (containing inorganic salts, excess solvent, etc.) separate into layers. In the post-processing stage S5, the water is separated by heating to 80°C. The difference in boiling points between the organic phase and water is used to evaporate the water and then condense it to reduce solvent residue in the product. When the temperature is raised to 120°C, the residual trace water is completely removed to ensure product purity. At the same time, the aqueous layer is reused in the sodium cyanide preparation vessel to achieve resource recycling and reduce wastewater treatment costs. The entire process achieves low-cost and high-efficiency synthesis of N,N-diisopropylaminoacetonitrile through raw material ratio optimization and step-by-step reaction control.

[0028] This invention avoids the use of expensive chloroacetonitrile reaction, greatly reducing production costs. It is easy to operate, requires no complicated refining process, effectively reduces the difficulty of production and refining of the product, meets environmental protection requirements, and is conducive to its widespread application in production.

[0029] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0030] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for synthesizing N,N-diisopropylaminoacetonitrile, characterized in that, The synthesis materials include the following: diisopropylamine, formaldehyde, sodium cyanide, hydrochloric acid, and water, wherein the molar ratio of diisopropylamine, formaldehyde, and sodium cyanide is 1:1.1:

1.

2. A process for synthesizing N,N-diisopropylaminoacetonitrile, characterized in that, The synthesis of N,N-diisopropylaminoacetonitrile according to claim 1 includes the following steps: S1. Equipment required for synthesis: 2 x 50L reactors, 1 x 100L reactor, 1 x 3㎡ condenser, 1 x 1L glass water separator, 1 x integrated heating and cooling unit, 1 x water circulation vacuum pump, and 1 x 5L receiving bottle. S2. Check the equipment: Check the sealing condition to ensure normal use, wear appropriate personal protective equipment, and rinse all tools with 3% sodium hypochlorite before use; S3. Preparation of sodium cyanide aqueous solution: Add 5 kg of sodium cyanide to a 50 L reactor, vacuum pump in 30 kg of water, stir to dissolve and obtain sodium cyanide aqueous solution for later use. S4. Main reaction stage: First, vacuum pump 25.82 kg of 40% diisopropylamine and 8.27 kg of 37% formaldehyde into a 100L reactor. Cool to 10℃, add 2 kg of hydrochloric acid to the dropping funnel, and add it dropwise into the 100L reactor. Adjust the pH to 10 and finish the addition after 2 hours. Then, add the prepared sodium cyanide aqueous solution dropwise and finish the addition after 2 hours. Keep the temperature at 20℃ for 2 hours, let it stand for about 30 minutes, separate the lower water layer, let the water layer stand and transfer it to the wastewater treatment vessel. After washing with sodium hypochlorite and testing with cyanide test paper, transfer it to the sewage treatment plant after it passes the test. S5. Post-processing of the product: The upper organic phase is transferred to the dehydration kettle. The temperature is raised to 80°C to start the separation of water. The organic layer is condensed by the condenser and then flows back to the reaction kettle through the water separator. The water layer is condensed by the condenser and then flows to the lower layer of the water separator to the receiving bottle. It is then transferred to the sodium cyanide preparation kettle. The process ends when the temperature rises to 120°C. The material is then discharged and packed into barrels.

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