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Method for preparing 2,2-diisopropylpropionitrile

A technology for propylpropionitrile and propionitrile, which is applied in the field of preparing 2,2-diisopropylpropionitrile, can solve the problems of harsh production conditions, unfavorable industrial operation, expensive raw materials and the like, achieves short production cycle and is beneficial to industrialization The effect of simple production and reaction process

Inactive Publication Date: 2013-09-11
WENZHOU ZHONGTAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] For this reason, the technical problem to be solved by the present invention lies in the problems of expensive raw materials, harsh production conditions, long production cycle and unfavorable industrial operation in the prior art, thereby providing a kind of low production cost, simple production process and long production cycle. The method for preparing 2,2-diisopropylpropionitrile which is short and beneficial to industrialized production

Method used

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  • Method for preparing 2,2-diisopropylpropionitrile
  • Method for preparing 2,2-diisopropylpropionitrile
  • Method for preparing 2,2-diisopropylpropionitrile

Examples

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Embodiment 1

[0033] Using isopropyl alcohol and methanesulfonyl chloride as raw materials to prepare isopropylsulfonate, the isopropylsulfonate and propionitrile prepare 2,2-diisopropylpropionitrile under the catalysis of strong base lithium amide. R in the isopropyl sulfonate is a methyl group, and its chemical reaction formula is:

[0034] .

[0035] The preparation steps are: (1) Dissolve 11.5g (0.1mol) of methanesulfonyl chloride in 50ml of pyridine solvent, slowly add 6.0g (0.1mol) of isopropanol dropwise at room temperature, and keep stirring for 2 hours to make it react;

[0036](2) Recover the solvent under reduced pressure, dissolve the resulting residue in 30ml of ethyl acetate to obtain an ester layer, wash the ester layer with water, dry the ester layer with anhydrous sodium sulfate, remove ethyl acetate under reduced pressure to obtain isopropyl methanesulfonate Ester crude product 13.0g, yield is 94.2%, described isopropyl mesylate crude product does not need purification,...

Embodiment 2

[0040] Using isopropyl alcohol and benzene methanesulfonyl chloride as raw materials to prepare isopropyl sulfonate, said isopropyl sulfonate and propionitrile prepare 2,2-diisopropylpropionitrile under the catalysis of strong alkali calcium hydride, R in the isopropyl sulfonate is benzyl, and its chemical reaction formula is:

[0041] .

[0042] The preparation steps are: (1) Dissolve 17.5g (0.1mol) of benzenemethanesulfonyl chloride in 60ml of pyridine solvent, slowly add 6.0g (0.1mol) of isopropanol dropwise at room temperature, and keep stirring for 5 hours to make it react ;

[0043] (2) Recover the solvent under reduced pressure, dissolve the resulting residue in 40ml of ethyl acetate to obtain an ester layer, wash the ester layer with water, dry the ester layer with anhydrous sodium sulfate, and remove ethyl acetate under reduced pressure to obtain isobenzenemethanesulfonate Propyl ester crude product 17.2g, yield 86.0%, described isopropyl benzene methanesulfonate ...

Embodiment 3

[0047] Using isopropyl alcohol and trifluoromethanesulfonyl chloride as raw materials to prepare isopropylsulfonate, the isopropylsulfonate and propionitrile are catalyzed by strong base sodium ethoxide to prepare 2,2-diisopropylpropionitrile , R in the isopropylsulfonate is trifluoromethyl, and its chemical reaction formula is:

[0048] .

[0049] The preparation steps are: (1) Dissolve 16.8g (0.1mol) of trifluoromethanesulfonyl chloride in 40ml of pyridine solvent, slowly add 6.0g (0.1mol) of isopropanol dropwise at room temperature, and keep stirring for 3 hours to make it reaction;

[0050] (2) Recover the solvent under reduced pressure, dissolve the resulting residue in 30ml of ethyl acetate to obtain an ester layer, wash the ester layer with water, dry the ester layer with anhydrous sodium sulfate, and remove ethyl acetate under reduced pressure to obtain trifluoromethanesulfonic acid Isopropyl ester crude product 18.4g, yield is 95.8%, described isopropyl trifluorom...

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Abstract

The invention relates to a method for preparing 2,2-diisopropylpropionitrile, which comprises the following steps: preparing isopropyl sulfonic acid ester from isopropanol and sulfonyl chloride, and preparing the 2,2-diisopropylpropionitrile from the isopropyl sulfonic acid ester and propionitrile under the catalytic action of strong base. The invention solves the problems of high cost of raw materials, tough production conditions and long production cycle, and the problem that the method is not beneficial to industrial operation in the prior art. Thus, the method for preparing 2,2-diisopropylpropionitrile has the advantages of low production cost, simple production process and short production cycle, and is beneficial to industrial production.

Description

technical field [0001] The invention relates to a method for preparing 2,2-diisopropylpropionitrile. Specifically, it is a method for preparing 2,2-diisopropylpropionitrile with low production cost, simple production process, short production period and favorable industrial production. Background technique [0002] 2,2-Diisopropylpropionitrile is the key intermediate of the new cooling agent WS-23, the full name of WS-23 is N,2,3-trimethyl-2-(1-methyl Ethyl) butyramide or N,2,3-trimethyl-2-isopropyl butanamide is widely used in food, beverage, candy, cosmetics, tobacco products, medicine, etc. [0003] The preparation method of 2,2-diisopropylpropionitrile mainly contains two kinds at present, method one: the people such as Simeon adopts in the system of lithium diisopropylamide / tetrahydrofuran, methyl bromide and 2,2-diisopropyl condensed acetonitrile to synthesize 2,2-diisopropylpropionitrile; or in the presence of sodium amide / liquid ammonia, condensed methyl iodide and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/03C07C253/30
Inventor 王凯王平
Owner WENZHOU ZHONGTAI CHEM
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