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Method for synthesizing high-content allyl isothiocyanate

A technology of allyl isothiocyanate and synthesis method, applied in the direction of organic chemistry, etc., can solve the problems of low extract content and long cultivation period

Inactive Publication Date: 2012-05-16
徐波勇 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is a method for extracting allyl isothiocyanate from horseradish in China. This method requires a long period of cultivation to obtain the finished product, and the content of the extract is low; there are reports of synthetic isothiocyanate in China, but the yields of each method are low. Not more than 95.5%, the content is not more than 95%

Method used

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  • Method for synthesizing high-content allyl isothiocyanate
  • Method for synthesizing high-content allyl isothiocyanate
  • Method for synthesizing high-content allyl isothiocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Take 12.1 g of allyl bromide, add it to 200 ml of acetonitrile, then add 9.7 g of potassium hydrosulfide, stir in a water bath, control the temperature at 10-20°C, add 0.1 g of trioctylmethyl ammonium chloride after 5 minutes, and raise the temperature to 30°C, heat-preserve at 30-40°C for reaction, filter with suction after 1 hour, and distill the filtrate under atmospheric pressure to obtain allyl isothiocyanate with a yield of 98.1%.

Embodiment 2

[0010] Take 12.1 grams of allyl bromide, add it to 200 ml of acetonitrile, then add 9.7 grams of potassium hydrosulfide, stir in a water bath, control the temperature at 20 ° C, add 0.05 g of trioctylmethyl ammonium chloride after 5 minutes, and heat up to 50 ℃, heat preservation reaction at 50-55 ℃, suction filtration after 1 hour, and atmospheric distillation of the filtrate to obtain allyl isothiocyanate with a yield of 98.9%.

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Abstract

The invention discloses a method for synthesizing high-content allyl isothiocyanate. The allyl isothiocyanate has bactericidal activity, and can be taken as a fumigant instead of curafume. In the method, methyl trioctyl ammonium chloride is taken as a phase transfer catalyst for use in an allyl isothiocyanate synthesis reaction, so that reaction time is shortened to 1.4 hours, and the reaction yield is increased by 98.9 percent; and acetonitrile is taken as a reaction solvent, and allyl bromide reacts with potassium rhodanate, so that allyl isothiocyanate of which the content is over 98 percent is finally synthesized.

Description

Technical field: [0001] The invention discloses a method for synthesizing high-content allyl isothiocyanate, which belongs to the field of chemical synthesis. Allyl isothiocyanate has fungicidal activity and can replace methyl bromide as a fumigant. Background technique: [0002] For a long time, phosphine and methyl bromide have been used as the main chemical fumigants for storage pest control, but there are still many problems with these fumigants. Studies have shown that storage pests have developed high resistance to phosphine, and because methyl bromide is considered one of the reasons for the destruction of the ozone layer, the Montreal Protocol (1997) has stipulated that developed countries should ban methyl bromide in 2005 and developing countries in 2015 usage of. [0003] Allyl isothiocyanate is an important chemical product. It has been reported at home and abroad that allyl isothiocyanate has the potential to replace methyl bromide in some aspects. There is a ...

Claims

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Application Information

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IPC IPC(8): C07C331/22
Inventor 徐波勇孙建亮方文胜高明强吕胜春范飞飞王磊磊
Owner 徐波勇
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