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Method for synthesizing phenyl isothiocyanate

A technology of phenyl isothiocyanate and synthetic method, which is applied in the direction of organic chemistry, can solve the problems of being unsuitable for large-scale industrial production, large environmental impact, long production cycle, etc., and achieves the convenience of industrial production, short reaction cycle, The effect of low production cost

Active Publication Date: 2014-04-30
ZHEJIANG BULK CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] These methods have disadvantages such as long production cycle, high risk, and great impact on the environment to varying degrees, and are not suitable for large-scale industrial production.

Method used

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  • Method for synthesizing phenyl isothiocyanate
  • Method for synthesizing phenyl isothiocyanate
  • Method for synthesizing phenyl isothiocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Add 7.2 kg of deionized water to a reactor, add 1 kg of aniline, and start stirring, then add 2.7 kg of tetramethylthiuram disulfide; heat the reactor to 90°C-100°C and reflux for 4 hours, Stop heating, lower the temperature of the reactor to 70°C-80°C, add 3.3kg of 30% hydrochloric acid, then raise the temperature to 90°C-100°C and reflux for 4 hours, then cool to room temperature.

[0037] (2) Centrifuge to separate the sulfur, wash the sulfur with 0.36kg of petroleum ether, and petroleum ether is used to extract the water phase after separating the oil layer. The acidic aqueous phase was distilled to dryness to obtain dimethylamine hydrochloride. The liquid phase separated by centrifugation was statically separated, the lower oil phase was 1.97 kg of crude phenyl isothiocyanate, the upper aqueous phase was extracted with washed petroleum ether, and the oil phase and petroleum ether solvent were combined.

[0038] (3) The above-mentioned phenyl isothiocyanate cru...

Embodiment 2

[0050] (1) Add 7.2 kg of deionized water to a reactor, add 1 kg of aniline, and start stirring, then add 2.5 kg of tetramethylthiuram disulfide; heat the reactor to 90°C-100°C and reflux for 4 hours, Stop heating, lower the temperature of the reactor to 70°C-80°C, add 3.0kg of 30% hydrochloric acid, then raise the temperature to 90°C-100°C and reflux for 4 hours, then cool to room temperature.

[0051] (2) Centrifuge to separate the sulfur, wash the sulfur with 0.35kg of petroleum ether, and petroleum ether is used to extract the water phase after separating the oil layer. The acidic aqueous phase was distilled to dryness to obtain dimethylamine hydrochloride. The liquid phase separated by centrifugation was allowed to stand for stratification, the lower oil phase was 1.86 kg of crude phenyl isothiocyanate, the upper water phase was extracted with washed petroleum ether, and the oil phase and petroleum ether solvent were combined.

[0052] (3) The crude product of phenyl isot...

Embodiment 3

[0054] (1) Add 7.2 kg of deionized water to a reaction kettle, add 1 kg of aniline, and start stirring, then add 3.0 kg of tetramethylthiuram disulfide; heat the reaction kettle to 90°C-100°C and reflux for 4 hours, Stop heating, lower the temperature of the reactor to 70°C-80°C, add 3.5kg of 30% hydrochloric acid, then raise the temperature to 90°C-100°C and reflux for 4 hours, then cool to room temperature.

[0055] (2) Centrifuge to separate the sulfur, wash the sulfur with 0.40kg of petroleum ether, and petroleum ether is used to extract the water phase after separating the oil layer. The acidic aqueous phase was distilled to dryness to obtain dimethylamine hydrochloride. The liquid phase separated by centrifugation was allowed to stand for stratification, and the lower oil phase was 2.01 kg of crude phenyl isothiocyanate. The upper aqueous phase was extracted with washed petroleum ether, and the oil phase and petroleum ether solvent were combined.

[0056] (3) The crude ...

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Abstract

The invention discloses a method for synthesizing phenyl isothiocyanate. The method comprises the following steps: (1) heating aniline and tetramethyl thiuram disulfide in water to react so as to obtain a reaction liquid A after the reaction is finished; (2) performing salt forming reaction between the reaction liquid A obtained in the step 1 and acid, and after the reaction is finished, performing centrifugal separation to obtain a solution B and solids; (3) extracting the solution B obtained in the step (2) by using an organic solvent so as to obtain water phase and organic phase, evaporating the water phase to obtain salt of dimethylamine, and performing posttreatment on the organic phase to obtain the phenyl isothiocyanate. The synthesis method is simple to operate, phenyl isothiocyanate is generated in one step and the sulfur and dimethylamine salt generated in the production process can be used as byproducts without being discharged, so that the synthesis process is free of pollution to the environment.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing phenyl isothiocyanate. Background technique [0002] Phenyl isothiocyanate, whose structure is shown in formula (I), has stronger biological activity than isothiocyanate, and is mainly used in pesticides, medicines, dyes, and biochemical research. Phenyl isothiocyanate can react with hydrazide to prepare a series of thiourea and related organic compounds, and these compounds have strong activity. It is mostly used to synthesize various types of heterocyclic compounds, such as antibacterial, anti-inflammatory and cancer treatment in medicine; it is used as antibacterial, insecticide, herbicide, etc. in pesticides; at the same time, they can also be used to determine peptides and amino acid sequences in proteins and as fluorescein markers. [0003] [0004] In the prior art, the method for synthesizing phenylisothiocyanate mainly contains the followin...

Claims

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Application Information

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IPC IPC(8): C07C331/28
Inventor 李加尧陈江平傅桂萍
Owner ZHEJIANG BULK CHEM
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