Preparation method of 2,3-dimethyl-2-isopropyl butyronitrile

A technology of propyl butyronitrile and dimethyl, applied in 2, to achieve the effect of reducing cost, high yield and good product quality

Inactive Publication Date: 2010-09-08
JIANGSU GRANDCHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the increasing demand for WS-23, the demand for 2,3-dimethyl-2-isopropylbutyronitrile is also increasing, but no domestic manufacturers can stably produce this product in batches

Method used

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  • Preparation method of 2,3-dimethyl-2-isopropyl butyronitrile

Examples

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preparation example Construction

[0014] A kind of 2, the preparation method of 3-dimethyl-2-isopropylbutyronitrile of the present invention comprises the steps:

[0015] The first step is to cool the ammonia gas to a liquid state and add it to the low-temperature reaction kettle, then add sodium amide, start stirring to mix the materials in the kettle evenly, and adjust the temperature in the low-temperature reaction kettle to -40~-70°C; the liquid in the above process Ammonia is a solvent, and sodium amide is an alkali, and their respective weight percentages are respectively 30-40% and 10-18% of the reaction mixture solution.

[0016] In the second step, propionitrile and 2-bromopropane are added into a high-position stirring dropping tank and mixed evenly; the weight percentages of propionitrile and 2-bromopropane are respectively 6-10% and 35-45%.

[0017] In the third step, slowly drop the mixed liquid obtained in the second step into the low-temperature reaction kettle, adjust the temperature in the low...

Embodiment 1

[0021] First use low-temperature cooling, cool 800 kg of liquid ammonia and add it to a 3000L low-temperature reaction kettle, then add 350 kg of sodium amide, start stirring to make the kettle evenly stirred. Maintain the temperature in the reactor between -50 and -60°C. Add 150 kg of propionitrile and 850 kg of 2-bromopropane into the high-position stirring drop tank, and stir evenly. Then slowly drop the mixed solution into the low-temperature reactor, the dropping process is strongly exothermic, and the temperature in the reactor must be controlled not to be higher than -50°C during the dropping process. The dropwise addition time is 8 hours, after the dropwise addition is completed, the temperature is kept at low temperature for 10 hours, and the reaction temperature is set at about -50 degrees. After the reaction is completely finished, the liquid ammonia is recovered by evaporation, and the evaporation ends in about 2-4 hours. 100 kg of water was added dropwise to que...

Embodiment 2

[0023] First use low-temperature cooling, cool 800 kg of liquid ammonia and add it to a 3000L low-temperature reaction kettle, then add 350 kg of sodium amide, start stirring to make the kettle evenly stirred. Maintain the temperature in the reactor between -40. Add 150 kg of propionitrile and 850 kg of 2-bromopropane into the high-position stirring drop tank, and stir evenly. Then slowly drop this mixed solution into the low-temperature reaction kettle. During the dropping process, the heat is strongly exothermic. Be sure to control the temperature in the reaction kettle during the dropping process not to be higher than -40°C. The dropwise addition time is 8 hours, after the dropwise addition is completed, the temperature is kept at low temperature for 6 hours, and the reaction temperature is set at about -40 degrees. After the reaction is completely finished, the liquid ammonia is recovered by evaporation, and the evaporation ends in about 2-4 hours. Water was added dropwi...

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Abstract

The invention discloses a preparation method of 2,3-dimethyl-2-isopropyl butyronitrile. The preparation method comprises the following steps of: firstly, cooling ammonia to a liquid state, adding obtained liquid ammonia into a low-temperature reaction kettle and then adding sodamide; secondly, adding propionitrile and 2-bromopropane into a high-order stirring and dropping pot and uniformly mixing; next, slowly dropping a mixed liquor obtained in the second step into the low-temperature reaction kettle, regulating the temperature in the low-temperature reaction kettle, and after complete reaction, evaporating and recovering the liquid ammonia; and finally, adding ethyl acetate to extract a water phase in the third step, respectively washing the water phase by using clear water and a saline solution, drying, filtering and desolventizing a final organic phase and distilling in vacuum to prepare the 2,3-dimethyl-2-isopropyl butyronitrile after the desolventizing. The method has scientific material selection, proper proportioning and simplicity and is suitable for industrial production. Moreover, the reaction time is short, the yield is high, and the quality of the product is good.

Description

technical field [0001] The invention belongs to the technology used as a precursor raw material of novel synthetic cooling agent WS-23 (N, 2, 3-trimethyl-2-isopropylbutyramide) and as a monomer fragrance, especially a kind of 2, The preparation method of 3-dimethyl-2-isopropylbutyronitrile. Background technique [0002] With the development of the economy and the improvement of people's living standards and consumption levels, consumers' demand for food and requirements for food taste are also getting higher and higher. Therefore, the demand for cooling agents as one of the food additives is also expanding, the demand in foreign markets is expanding day by day, and the demand in domestic market is also expanding. [0003] Research on the physiological cooling of the human body began in the 1970s. In 1970, under the leadership of Roy Randolph, Wilkinson Sword Ltd carried out extensive research on this subject. Only WS-3 (N-ethyl-p-menthyl-3-carboxamide) and WS-23 (N,2,3-tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/03C07C253/30
Inventor 赵学飞蒋世明
Owner JIANGSU GRANDCHEM IND
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