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Acetylthiocholine iodide as well as preparation method and application thereof

A technology of iodothioacetylcholine and thioacetic acid, which is applied in the direction of analyzing materials through chemical reactions, observing the influence of chemical indicators on materials, organic chemistry, etc., can solve unfavorable industrial production, intermediates, etc. Harsh conditions, unstable raw materials and other problems, to achieve the effect of excellent clarity, easy to obtain raw materials, and low cost

Inactive Publication Date: 2019-06-14
安徽昊帆生物有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] However, this route is not only difficult to obtain raw materials, but also the raw materials themselves are very unstable, and the conditions for the addition reaction of the obtained intermediates are harsh, and the yield is low, which is not conducive to industrial production

Method used

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  • Acetylthiocholine iodide as well as preparation method and application thereof
  • Acetylthiocholine iodide as well as preparation method and application thereof
  • Acetylthiocholine iodide as well as preparation method and application thereof

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preparation example Construction

[0038] The preparation method of the iodothioacetylcholine according to the embodiment of the present invention comprises the following steps:

[0039] Step S1, providing an aqueous alkaline solution obtained by dissolving dimethylaminoethane compounds in alkali.

[0040] Wherein, the dimethylaminoethane compound refers to dimethylaminoethane and its derivatives, specifically, may include dimethylaminoethane, dimethylaminochloroethane, dimethylaminobromoethane, or a mixture thereof , wherein, preferably dimethylaminobromoethane.

[0041] The base is not particularly limited, for example, it can be an organic base or an inorganic base, preferably an inorganic base, such as sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium hydroxide, potassium hydroxide, or a mixture thereof.

[0042] Step S2, adding a thioacetic acid compound to the alkaline aqueous solution to cause a thio reaction with the dimethylaminoethyl compound to generate dimethy...

Embodiment 1

[0066] In a 5L three-necked flask, take by weighing 121.6g of potassium carbonate and place in the bottle, add 1.5L of water, stir and dissolve, then add 150.8g of dimethylaminobromoethane hydrochloride to it, make it all free, and get a clear solution. Cool down to 5-10°C in an ice-salt bath, add 136.8g potassium thioacetate to the bottle, after the addition is complete, stir at room temperature (25°C) for 6 hours, during which time the solid state of the system and the color of the system will change from white to brown.

[0067] After completion of the reaction, add 2L ethyl acetate to the system, extract and separate the liquids, and the obtained organic phase is dried with anhydrous magnesium sulfate, suction filtered, and the filtrate is concentrated to obtain intermediate dimethylaminoethyl thioacetic acid 130g.

[0068] Into a 2L three-necked flask, add 130g of the above-mentioned intermediate and 1.3L of tetrahydrofuran, control the temperature, and add 144.6g of methy...

Embodiment 2

[0075] In a 5L three-neck flask, weigh 17.6g of sodium hydroxide and place it in the bottle, add 1.5L of water, stir to dissolve, then add 150.8g of dimethylaminobromoethane hydrochloride to it, make it all free, and obtain a clear solution . Cool down to 5-10°C in an ice-salt bath, add 136.8g potassium thioacetate to the bottle, after the addition is complete, stir at room temperature (25°C) for 6 hours, during which the solid state and color of the system will change from white to brown.

[0076] After completion of the reaction, add 2L ethyl acetate to the system, extract and separate the liquids, and the obtained organic phase is dried with anhydrous magnesium sulfate, suction filtered, and the filtrate is concentrated to obtain intermediate dimethylaminoethyl thioacetic acid 120g.

[0077] Into a 2L three-necked flask, add 120g of the above-mentioned intermediate and 1.2L of tetrahydrofuran, control the temperature, and add 133.5g of methyl iodide dropwise at about 20°C, ...

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Abstract

The invention provides acetylthiocholine iodide and a preparation method thereof. The preparation method comprises the following steps: step S1, dissolving a dimethylamino ethane compound in alkali toobtain an alkaline aqueous solution; step S2, adding a thioacetic acid compound into the alkaline aqueous solution to subject the thioacetic acid compound and the dimethylamino ethane compound to a thioreaction to generate (2-(dimethylamino)ethyl)ethanethioate; S3, separating the (2-(dimethylamino)ethyl)ethanethioate, and preparing an organic solution of the (2-(dimethylamino)ethyl)ethanethioate;and S4, dropwise adding an organic iodide into the organic solution of the (2-(dimethylamino)ethyl)ethanethioate for an iodination reaction so as to generate the acetylthiocholine iodide. According to the preparation method provided by the embodiment of the invention, the high-purity acetylthiocholine iodide can be obtained, and the titration content, the melting point, the clarity and other dataof the product are very excellent. The method is simple in operation, good in safety, suitable for industrial production, easy in raw material obtaining and low in cost.

Description

technical field [0001] The invention belongs to the chemical synthesis of medicines in the field of organic chemistry, and specifically relates to iodothioacetylcholine, its preparation method, and its application. Background technique [0002] Food safety has become a hot issue in the current society. Severely excessive pesticide residues can cause acute poisoning, and the long-term accumulation and retention of minor pesticide residues in the human body can also cause many chronic diseases. Therefore, how to detect organophosphorus and carbamate pesticide residues in fruits and vegetables simply, quickly and accurately is particularly important. Acetylcholinesterase (AChE) can selectively catalyze the hydrolysis of substrates, and its catalytic activity can be inhibited by organophosphate or carbamate pesticides. This feature can be used to make a biosensor for rapid determination of organophosphorus pesticide content, substrate content and enzyme activity. [0003] Iod...

Claims

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Application Information

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IPC IPC(8): C07C327/30G01N21/78
Inventor 孙豪义孙跃顾耿峰
Owner 安徽昊帆生物有限公司
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