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Method for synthesizing m-phenoxybenzoic cyanohydrin ester succinate

A technology of m-phenoxybenzocyanohydrin succinate and m-phenoxybenzocyanhydrin, which is applied in chemical instruments and methods, preparation of carboxylic acid nitriles, preparation of organic compounds, etc., to achieve simple synthesis steps Effect

Inactive Publication Date: 2008-04-09
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Up to now, there is no enzyme-linked immunoassay report on derivatives synthesized by pyrethroid intermediate m-phenoxybenzocyanohydrin at home and abroad. In order to make up for this gap, it is necessary to synthesize m-phenoxybenzocyanhydrin Derivatives

Method used

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  • Method for synthesizing m-phenoxybenzoic cyanohydrin ester succinate
  • Method for synthesizing m-phenoxybenzoic cyanohydrin ester succinate

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Embodiment 1

[0019] (1) the preparation of m-phenoxybenzoyl cyanohydrin:

[0020] Add 0.3g (4.6mmol) potassium cyanide and 1ml distilled water in a small reaction flask equipped with a stirrer, cool to -15°C under stirring, add m-phenoxybenzaldehyde 0.8g (4.0mmol), in 1 ml (5.3 mmol) of 40% sulfuric acid was added dropwise within 10 minutes. After continuing to stir for 15 minutes, it was extracted with 40 ml of carbon tetrachloride. After the extract was dried with anhydrous sodium sulfate, the solvent was removed to obtain 0.64g (2.9mmol) of m-phenoxybenzyl cyanohydrin, n D = 1.5823.

[0021] (2) Synthesis of the derivative m-phenoxybenzocyanhydrin succinate of m-phenoxybenzocyanhydrin:

[0022] Dissolve the obtained m-phenoxybenzocyanohydrin in 10 mL of anhydrous pyridine, then add 0.35 g (3.5 mmol) of succinic anhydride, heat in a sand bath to 130 ° C, reflux for 3 hours under magnetic stirring, and then cool with ice water The reactor was removed from the solvent, and then washed ...

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Abstract

The invention relates to a synthetic method for m-phenoxybenzoic armour cyanhydrin succinic acid ester, and belongs to the technical field of biochemistry industry. By utilizing m-Phenoxybenzaldehyde as the raw material, the synthetic method includes two steps of reactions including compounding m-phenoxy armour cyanhydrin primarily and compounding the m-phenoxybenzoic armour cyanhydrin succinic acid ester subsequently. By utilizing simple synthetic processes, the invention successfully compounds the m-phenoxybenzoic armour cyanhydrin succinic acid ester which is a derivate of the m-phenoxy armour cyanhydrin. After the post treatment, the m-phenoxybenzoic armour cyanhydrin succinic acid ester with a purity of more than 99 precent can be used as standard. The invention provides a convenient way for future test and research on the enzyme-linked immunoassay of pyrethroids containing cyano group, and satisfies the needs of the relative researchers both domestic and abroad.

Description

technical field [0001] The invention discloses a method for synthesizing m-phenoxybenzyl cyanohydrin succinate, which belongs to the technical field of biochemical industry. Background technique [0002] m-phenoxybenzocyanohydrin, English name: 3-Phenoxybenzoaldehyde cyanohydrin, molecular formula is C 14 h 11 NO 2 , is an intermediate in the synthesis of cyano-containing pyrethroid pesticides. Pyrethroids are a class of biomimetic drugs developed on the basis of the chemical structure of natural pyrethroids. The application of natural pyrethrum has a long history. Because of its strong knockdown power, fast insecticidal effect, broad spectrum, easy degradation, low toxicity to higher animals and birds, safe use, and little environmental pollution, it is widely used Widely used in tea gardens, orchards, farmland and other pest control. With the improvement of international standards, the internationalization of my country's trade, and the strict green barriers, the prob...

Claims

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Application Information

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IPC IPC(8): C07C255/38C07C253/30
Inventor 胥传来郝晓蕾陶冠军秦昉
Owner JIANGNAN UNIV
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