Synthetic method for efficiently preparing folcisteine

A synthesis method and a technology for halifolin, applied in the direction of organic chemistry and the like, can solve the problems of complex process route, high production cost, poor product quality, etc., and achieve the effects of improving reaction yield, yield improvement and good crystal form.

Inactive Publication Date: 2018-12-21
CHENGDU BAISHIXING SCI & TECH IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the defects of complex process route, high production cost, low yield and poor product quality in the above-mentioned prior art, the present invention provides a simple and efficient process for synthesizing hemiphyllin that can overcome the existing technical drawbacks method

Method used

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  • Synthetic method for efficiently preparing folcisteine

Examples

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Effect test

experiment example 1

[0031] Add 300 kilograms of tap water, 92 kilograms of 37% formaldehyde solution and 100 kilograms of L-cysteine ​​hydrochloride monohydrate in a 500-liter reactor. Within the range of 7-10, after the reaction of the raw materials is detected by pointing the plate, the temperature is raised to 50°C, and acetic anhydride and saturated sodium carbonate solution are added dropwise at the same time to maintain the pH value of the reaction system within the range of 7-10. After the addition is completed, the reaction is continued for 1 After 1 hour, point the plate to detect that the raw materials have reacted completely, add concentrated hydrochloric acid dropwise, adjust the pH of the system to 5-6, add 20 kg of activated carbon, heat and decolorize, beat the plate frame to reflux and filter, add concentrated hydrochloric acid dropwise to the filtrate to adjust the pH to 1-2, Under slow stirring, the temperature was lowered for crystallization, the precipitated solid was centrifug...

experiment example 2

[0034] Add 300 kilograms of tap water, 50 kilograms of 37% formaldehyde solution and 100 kilograms of L-cysteine ​​hydrochloride monohydrate in a 500-liter reactor, after stirring and clarifying at room temperature, add dropwise saturated sodium carbonate solution to maintain the pH value of the reaction system Within the range of 7-10, after the reaction of the raw materials is detected by pointing the plate, the temperature is raised to 50°C, and acetic anhydride and saturated sodium carbonate solution are added dropwise at the same time to maintain the pH value of the reaction system within the range of 7-10. After the addition is completed, the reaction is continued for 1 After 1 hour, point the plate to detect that the raw materials have reacted completely, add concentrated hydrochloric acid dropwise, adjust the pH of the system to 5-6, add 20 kg of activated carbon, heat and decolorize, beat the plate frame to reflux and filter, add concentrated hydrochloric acid dropwise ...

experiment example 3

[0037] Add 280 kilograms of tap water, 48 kilograms of 37% formaldehyde solution and 100 kilograms of L-cysteine ​​hydrochloride monohydrate in a 500-liter reactor. Within the range of 7-10, after the reaction of the raw materials is detected by pointing the plate, the temperature is raised to 50°C, and acetic anhydride and saturated sodium carbonate solution are added dropwise at the same time to maintain the pH value of the reaction system within the range of 7-10. After the addition is completed, the reaction is continued for 1 Hour. After the reaction of the raw materials is completely detected by pointing the plate, add concentrated hydrochloric acid dropwise to adjust the pH of the system to 5-6, add 20 kg of activated carbon, heat and decolorize, beat the plate frame to reflux and filter, add concentrated hydrochloric acid to the filtrate to adjust the pH to 1-2, and stir slowly Next, cool down and crystallize. The precipitated solid was centrifuged, dried, and package...

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Abstract

The invention discloses a synthetic method for efficiently preparing folcisteine, belonging to the field of organic chemistry, comprising the following reaction steps: S1: reacting L-cysteine and 37%aqueous formaldehyde solution until L-cysteine is fully reacted to obtain L-thioproline; S2: directly adding an acetylation reagent to the system obtained by S1, and performing one-pot reaction untilL-thioproline is completely reacted; S3: adjusting the pH of the system obtained by S2 to 5-6, adding activated carbon for heating and decolorizing, cooling, adjusting the pH to 1-3, cooling and crystallizing to obtain folcisteine. The one-pot reaction is adopted for preparing acetyl thioproline, to avoid the post-treatment step of extracting intermediate thioproline after the first step reaction,shorten the process route, reduce the operation steps, and improve the work efficiency.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a synthetic method for efficiently preparing hemiphyllin. Background technique [0002] Folcisteine, referred to as ATCA, the English name is Folcisteine, the chemical name is N-acetyl-thioproline, acetylthioproline, 3-acetyl-4-tetrahydrothiazole carboxylic acid. Hemiferin is a biostimulant plant growth regulator widely used in agriculture, mainly for foliar spraying and root irrigation. According to the difference of use, the formula mainly includes: ATCA5% + folic acid 0.1% + water and ATCA5% + folic acid 0.1% + amino acid 9% + water. The research results show that in the production of crops, the use of organic green fertilizers compounded with half-leaf elements can significantly improve the quality and yield of crops, and avoid secondary pollution of food caused by chemical fertilizers. It is mainly reflected in: increasing the main micronutrient elements of cro...

Claims

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Application Information

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IPC IPC(8): C07D277/06
CPCC07D277/06
Inventor 石常青
Owner CHENGDU BAISHIXING SCI & TECH IND
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