Method for synthesizing 4,4,4-trifluoro-butyronitrile

A technology of trifluorobutyronitrile and synthesis method, which is applied in 4 fields, can solve problems such as restricting the large-scale development of downstream products and expensive production costs, and achieve the effects of less catalyst consumption, simple production equipment, and short process flow

Inactive Publication Date: 2013-05-29
JUHUA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the past, these derivatives of 4,4,4-trifluorobutyronitrile, such as acids, amides, esters or amines, were all obtained through complicated process routes, resulting in high production costs of these products, which limited the large-scale production of their downstream products. scale development

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 0.02mol of 18-crown-6, 0.15mol of sodium cyanide, 200ml of N,N'-dimethylformamide and 0.75mol of 3,3,3-trifluoro-1-chloropropane into a 0.5L reactor Afterwards, the reaction vessel was sealed. Stirring was started, the temperature of the reactor was raised to 120°C, and the reaction was carried out at a constant temperature for 2 hours. The reactant was filtered and rectified to obtain 4,4,4-trifluorobutyronitrile with a yield of 92% based on sodium cyanide.

Embodiment 2

[0017] Add 0.008mol of cetyltrimethylammonium chloride, 0.5mol of sodium cyanide, 200ml of dimethyl sulfoxide and 0.6mol of 3,3,3-trifluoro-1-chloropropane in a 0.5L reactor , Seal the reactor. Stirring was started, the temperature of the reactor was raised to 110° C., and the reaction was stopped after a constant temperature reaction for 3.5 hours. The reactant was filtered and rectified to obtain 4,4,4-trifluorobutyronitrile with a yield of 88% based on sodium cyanide.

Embodiment 3

[0019] Add 0.05mol tetramethylammonium bromide, 0.3mol sodium cyanide, 200ml dimethyl sulfoxide and 0.6mol 3,3,3-trifluoro-1-chloropropane in a 0.5L reactor, and seal the reactor . Stirring was started, the temperature of the reaction kettle was raised to 90° C., and the reaction was stopped after constant temperature reaction for 4 hours. The reactant was filtered and rectified to obtain 4,4,4-trifluorobutyronitrile with a yield of 89% based on sodium cyanide.

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Abstract

The invention discloses a method for synthesizing 4,4,4-trifluoro-butyronitrile. 3,3,3-trifluoro-1-chloropropane reacts with sodium cyanide or potassium cyanide in polar proton inert solvent in the presence of PTC (phase transfer catalyst) to synthesize 3,3,3-trifluoro-butyronitrile with reaction temperature being 20-150 DEG C, mol ratio of catalyst to 3,3,3-trifluoro-1-chloropropane being 0.005:1-0.2:1, mol ratio of 3,3,3-trifluoro-1-chloropropane to sodium cyanide or potassium cyanide being 10:1-1:1, and concentration of sodium cyanide or potassium cyanide in solvent being 0.1-5mol / L. The invention has the advantages of short process flow and low raw material cost.

Description

technical field [0001] The invention relates to a synthesis method of 4,4,4-trifluorobutyronitrile. Background technique [0002] The nitrile group in 4,4,4-trifluorobutyronitrile is a very active group, which can react with other substances to generate acids, amides, esters or amines. The derivatives of these 4,4,4-trifluorobutyronitrile The compounds are all important trifluoromethyl building block reagents, and are mainly used as raw materials for medicine, medicine synthesis and organic solvents. [0003] In the literature report, there is no mention of the synthetic method of 4,4,4-trifluorobutyronitrile. [0004] In the past, these derivatives of 4,4,4-trifluorobutyronitrile, such as acids, amides, esters or amines, were all obtained through complicated process routes, resulting in high production costs of these products, which limited the large-scale production of their downstream products. scale development. Contents of the invention [0005] The purpose of this...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/10C07C253/14
Inventor 周强吴庆周晓红吴周安
Owner JUHUA GRP
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