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Preparation method for 2,2-diisopropyl propionitrile

A technology of propylpropionitrile and propionitrile, which is applied in the field of precursor material 2 of cooling agent WS-23, can solve the problems of unfavorable safety production, long production cycle and low efficiency, and avoid strong corrosion and irritation , Reduce operation steps, improve production efficiency

Active Publication Date: 2013-08-14
APPLE FLAVOR & FRAGRANCE GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] For the reaction route of Method 1, the raw materials are easy to obtain and the reaction process is simple, but the reaction system of sodium amide / liquid ammonia belongs to ultra-low temperature conditions, and the production cycle is too long due to the long reaction time, and the production process consumes a lot of energy; Ammonia is highly corrosive and irritating, unfriendly to the environment, and has a very high rate of chemical accidents, which is not conducive to safe production
Although the second method solves the problem of the reaction system between liquid ammonia and sodium amide, the reaction steps are two steps, and the production process involves multiple use and recovery of different solvents. The operation process is cumbersome and the efficiency is not high; and the process uses sulfuryl chloride compounds , which is highly irritating and corrosive, and sulfonyl chloride compounds are not easy to recycle, and finally form useless waste, which does not meet the requirements of green chemistry

Method used

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  • Preparation method for 2,2-diisopropyl propionitrile
  • Preparation method for 2,2-diisopropyl propionitrile
  • Preparation method for 2,2-diisopropyl propionitrile

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Add 300g of diethyl ether into a 1000mL reaction flask, then add 50g of sodium hydride, start stirring to make it evenly stirred, and slowly heat to reflux. 33g of propionitrile and 100g of 2-chloropropane were mixed evenly and added to the dropping funnel, then the mixture was slowly added dropwise into the reaction flask, exothermic during the dropping process, and the reaction was controlled to slowly reflux at 35°C. The dropwise addition time was 3 hours, and after the dropwise addition was completed, reflux was continued at 35° C. for 15 hours. After the reaction is complete, add 50 g of water dropwise to quench excess sodium hydride, separate the organic phase, wash once with 50 g of pure water and saturated brine, separate the water phase, add 10 g of anhydrous sodium sulfate to the organic phase and dry for 3 hours, filter out Crystalline sodium sulfate, normal pressure reclaims solvent, then decompression distills out 75g 2,2 diisopropyl propionitrile, product ...

Embodiment 2

[0024] Add 300g of toluene into a 1000mL reaction flask, then add 40g of calcium hydride, start stirring to make it evenly stirred, and slowly heat to 110°C. 33g of propionitrile and 150g of 2-chloropropane were mixed evenly and added to the dropping funnel, and then the mixture was slowly added dropwise to the reaction flask, exothermic during the dropping process, and the reaction was controlled to slowly reflux at 110°C. The dropwise addition time was 7 hours, and after the dropwise addition was completed, reflux was continued at 110° C. for 20 hours. After the reaction is complete, add 50g of water dropwise to quench excess calcium hydride, separate the organic phase, wash once with 50g of pure water and saturated brine, separate the water phase, add 10g of anhydrous sodium sulfate to the organic phase and dry for 3 hours, filter out Crystallization sodium sulfate, normal pressure reclaims solvent, then decompression distills out 72g 2,2 diisopropyl propionitrile, product ...

Embodiment 3

[0026] Add 250g of dioxane into a 1000mL reaction flask, then add 65g of potassium hydride, start stirring to make it evenly stirred, and slowly heat to reflux. 33g of propionitrile and 240g of 2-iodopropane were mixed evenly and added to the dropping funnel, then the mixture was slowly added dropwise into the reaction flask, exothermic during the dropping process, and the reaction was controlled to slowly reflux at 101°C. The dropping time was 8 hours, and after the dropping was completed, reflux was continued at 101° C. for 10 hours. After the reaction is complete, add 50 g of water dropwise to quench excess potassium hydride, separate the organic phase, wash once with 50 g of pure water and saturated brine, separate the water phase, add 10 g of anhydrous sodium sulfate to the organic phase and dry for 3 hours, filter out Crystallization sodium sulfate, normal pressure reclaims solvent, then decompression distills out 70g 2,2 diisopropyl propionitrile, product is colorless a...

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Abstract

The invention discloses a preparation method for 2,2-diisopropyl propionitrile. Production of 2,2-diisopropyl propionitrile is realized efficiently in one step by co-functions of a strong alkali with an isopropyl halogenated hydrocarbon and propionitrile in an organic solvent. The method is efficient, green, low in cost, low in pollution and convenient for industrialized production. In a process disclosed by the invention, the organic solvent is used to replace liquid ammonia of a conventional process, and reaction conditions are changed from an ultralow temperature to a common conventional heating reaction, so that energy consumption is greatly reduced, strong corrosivity and stimulation of the liquid ammonia is prevented, and at the same time, security coefficients of the production is greatly increased. In the process disclosed by the invention, the organic solvent can be used as a reaction medium and as an extraction solvent after the reaction is finished, so that operation steps are reduced effectively and production efficiency is increased.

Description

technical field [0001] The present invention relates to a kind of cooling agent WS-23 (N,2,3-trimethyl-2-isopropyl butanamide) precursor material 2,2-diisopropylpropionitrile preparation method, specifically It is a method for industrial production and preparation of 2,2-diisopropylpropionitrile. Background technique [0002] 2,2-Diisopropylpropionitrile is the key intermediate of the new cooling agent WS-23, which is widely used in food, beverage, candy, cosmetics, tobacco products, medicine, etc. [0003] Currently, there are mainly two methods for preparing 2,2-diisopropylpropionitrile suitable for industrial production. Method 1: Patent document CN101823983A discloses a preparation method of 2,2-diisopropylpropionitrile, the specific steps are: in the mixed system of liquid ammonia and sodium amide, add propionitrile and 2-bromo Propane, and continue to react under cryogenic conditions to the end, evaporate and recover liquid ammonia after the reaction is complete, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/03C07C253/30
Inventor 孟宪乐朱为宏李劲友
Owner APPLE FLAVOR & FRAGRANCE GRP
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