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A kind of preparation method of high-purity Jinggang mycamine

A technology of Jinggangmycolamine and Jinggangmycolamine, which is applied in the field of new preparation of high-quality Jinggangmycolamine, can solve the problems of inability to large-scale production and huge separation cost.

Active Publication Date: 2019-10-29
杭州佳嘉乐生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the chemical structure of Jinggang mycamine and Jinggang mycamine differ only by one carbon-carbon double bond, the chemical properties are almost the same, which leads to the huge cost of separation of Jinggang mycamine or Jinggang mycamine, which cannot be produced on a large scale

Method used

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  • A kind of preparation method of high-purity Jinggang mycamine
  • A kind of preparation method of high-purity Jinggang mycamine
  • A kind of preparation method of high-purity Jinggang mycamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Add 100 g mycoylidene A, 80 g NBS and 500 mL deionized water into a 1000 mL flask, and stir and react at 25° C. for 4 h. After the reactant was diluted 10 times with water, the ion exchange column (D113, Hangzhou Zhengguang Resin Co., Ltd., 1500mL, NH 4 + type), washed with 5000mL deionized water, and then eluted with 4500mL of 0.5mol / L ammonia water, collected the mixture of Jinggangmycin and Jinggangmycin, concentrated to dryness under reduced pressure, and obtained 45.2g sample.

[0022] (2) Dissolve the mixture in 500mL of water and place it in a 1000-mL hydrogenation reactor. At the same time, put 5g of supported Pd catalyst (Konna New Materials (Hangzhou) Co., Ltd.), add hydrogen to a pressure of 5MPa, and react at 50°C 4h. After the reaction finishes, filter off the solid, dilute 10 times with deionized water and go to the ion exchange column (same as above), wash with 5000mL deionized water, then elute with 4500mL0.5mol / L ammonia water, collect the mixture...

Embodiment 2

[0024] (1) Add different amounts of mycoylidene amine A, 80 g of NBS and 500 mL of deionized water into a 1000 mL flask, and stir and react at 25° C. for 4 h. After the reactant was diluted 10 times with water, it was put on an ion exchange column (D113, Hangzhou Zhengguang Resin Co., Ltd., 1500mL, NH4+ type), washed with 5000mL deionized water, and then eluted with 4500mL 0.5mol / L ammonia water to collect Jinggangmycin The mixture of amine and mycoamine was concentrated to dryness under reduced pressure to obtain a 45.2 g sample. (2) Dissolve the mixture in 500mL of water and place it in a 1000-mL hydrogenation reactor. At the same time, put 5g of supported Pd catalyst (Konna New Materials (Hangzhou) Co., Ltd.), add hydrogen to a pressure of 5MPa, and react at 50°C 4h. After the reaction, filter off the solid, dilute it 10 times with deionized water and put it on the ion exchange column (same as above), wash with 5000mL deionized water, and then elute with 4500mL 0.5mol / L am...

Embodiment 3

[0028] According to the method of step (1) of Example 1, a mixture of Jinggang mycylamine and Jinggang mycamine was obtained, and the amount of hydrogenation reaction solvent was optimized. 45g of the above-mentioned mixture plus different amounts of water (100, 250, 500, 1000, 1500) were dissolved and placed in a hydrogenation reactor, and 5g of loaded Pd catalyst (Konna New Materials (Hangzhou) Co., Ltd.) was added at the same time. To a pressure of 5MPa, react at 50°C for 4h. After the reaction, filter off the solid, dilute it 10 times with deionized water and put it on the ion exchange column (same as above), wash with 5000mL deionized water, and then elute with 4500mL 0.5mol / L ammonia water to collect Jinggang mycamine and Jinggang mycamine The mixture of amines was concentrated under reduced pressure and dried in vacuum (45°C) to obtain a sample of Jinggangmycin, which was detected by HPLC. The specific results are shown in the following table:

[0029] Solven...

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Abstract

Validamine and valienamine are important chemical raw materials but have high separation cost and complex separation process. The invention discloses a preparation method validamine, which includes the steps of: 1) hydrolyzing validoxylamine A through an NBS chemical method by adding the validoxylamine A and NBS to water as a solvent according to certain molar ratio, and performing a reaction for 4 h at 25 DEG C; 2) carrying out adsorption separation to the reaction product through a weak-acidic cation exchange resin, and concentrating the product to obtain a mixture of the validamine and valienamine; 3) under catalysis by a heavy metal catalyst, performing hydrogenation to the mixture, performing adsorption separation to the reaction product through a weak-acidic cation exchange resin, concentrating the product, and vacuum-drying the concentrate to obtain a high-quality validamine sample.

Description

technical field [0001] The invention relates to a new preparation process of high-quality Jinggangmycin. Background technique [0002] Jinggangmycin is an aminoglycoside agricultural antibiotic independently developed and produced in my country. It is produced by the metabolism of Streptomyces hygroscopicus var. jinggangensis yen. It can effectively inhibit rice sheath blight. One of the antibiotics with the highest unit and one of the most important varieties of biological pesticides. [0003] Jinggangmycin has formed a biotechnology industry with high economic benefits in my country. If Jinggangmycin can be used as raw material to develop high value-added products, it will undoubtedly bring higher economic and social benefits. Jinggangmycin A removes D-glucose to obtain Jinggangmycin A (Validoxylamine A), and Jinggangmycin A breaks at different C-N bond positions to obtain Valienamine or Validamine . Jinggang mycamine and Jinggang mycamine have strong inhibitory effect ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/08C07C215/44
CPCC07C213/02C07C213/08C07C215/44
Inventor 陈小龙陆跃乐范永仙
Owner 杭州佳嘉乐生物技术有限公司
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