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Preparation method of 2,6-difluorobenzamide by utilizing rhodococcus ruber

A technology of difluorobenzamide and Rhodococcus erythrococcus, applied in the biological field, can solve problems such as high requirements for production equipment and production conditions, low conversion rate and selectivity of the method, and harsh reaction conditions of the production process, so as to reduce production costs, The effect of high substrate tolerance and fast reaction speed

Active Publication Date: 2014-01-15
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In summary, the current production of 2,6-difluorobenzamide has the following deficiencies: 1. Part of the production process has harsh reaction conditions, which require high production equipment and production conditions, which increases production costs; 2. The conversion rate of some methods And the selectivity is low, the separation and purification steps are complicated, and it is not suitable for industrial production

Method used

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  • Preparation method of 2,6-difluorobenzamide by utilizing rhodococcus ruber
  • Preparation method of 2,6-difluorobenzamide by utilizing rhodococcus ruber

Examples

Experimental program
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Embodiment 1

[0029] A kind of method utilizing Rhodococcus rubrum to prepare 2,6-difluorobenzamide, the preparation steps are:

[0030] (1) Seed and fermentation culture: inoculate the strain of Rhodococcus ruber (CGMCC3090) into the seed medium, culture at 180r / min, 30°C for 28h to obtain the seed culture medium, and transfer it to fresh fermentation medium with an inoculation amount of 3wt%. Culture medium, 180r / min, 28°C, cultured for 48h, to obtain bacterial fermentation liquid:

[0031] Seed medium: glycerol 10g / L, peptone 5g / L, malt powder 3g / L, yeast powder 3g / L, NaCl 1g / L, pH7.0;

[0032] Fermentation medium: glucose 20g / L, yeast powder 5g / L, MgSO 4 ·7H 2 O. KH 2 PO 4 、K 2 HPO 4 0.5g / L, urea 7g / L, NaCl 2g / L, CoCl 2 0.02g / L, sodium glutamate 1g / L, pH7.0. Among them, urea and inducer CoCl2 are sterilized separately for 3-5 minutes.

[0033] (2) Preparation of Rhodococcus Erythrococcus Suspension: Centrifuge the above bacterial fermentation liquid, remove the supernatant, and...

Embodiment 2

[0040] In the present embodiment, steps (1), (2) and (4) are all the same as in Example 1, and only step (3) is described below.

[0041] (3) Conversion of 2,6-difluorobenzonitrile: the concentration of substrate 2,6-difluorobenzonitrile is 1mol / L, the reaction volume is 10ml, the final concentration of Rhodococcus cells is 2.37g / L, and the final concentration of adding is 1% methanol, conversion system is 50mmol / LpH7.5KH 2 PO 4 -NaOH buffer solution, 30°C, 180r / min, after conversion for 3 hours, the pure product of 2,6-difluorobenzamide was prepared.

[0042] It is detected that the conversion rate of 2,6-difluorobenzonitrile in this step reaches 100%, and the selectivity to 2,6-difluorobenzamide is 100%.

Embodiment 3

[0044] In the present embodiment, steps (1), (2) and (4) are all the same as in Example 1, and only step (3) is described below.

[0045] (3) Conversion of 2,6-difluorobenzonitrile: the concentration of substrate 2,6-difluorobenzonitrile is 2.5mol / L, the reaction volume is 10ml, the final concentration of Rhodococcus cells is 2.37g / L, and 1% of Tween 80, the conversion system is 50mmol / LpH7.5KH 2 PO 4 -NaOH buffer solution, 30°C, 180r / min, after conversion for 24h, pure 2,6-difluorobenzamide was prepared.

[0046] It is detected that the conversion rate of 2,6-difluorobenzonitrile in this step reaches 100%, and the selectivity to 2,6-difluorobenzamide is 100%.

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Abstract

The invention relates to a preparation method of 2,6-difluorobenzamide by utilizing rhodococcus ruber. The method comprises the following steps: (1) fermentation and culture of seeds; (2) preparation of rhodococcus ruber suspension fluid; (3) conversion of 2,6-difluorobenzonitrile; (4) preparation of finished products. The invention provides a preparation method of 2,6-difluorobenzamide by utilizing rhodococcus ruber to convert 2,6-difluorobenzonitrile into 2,6-difluorobenzamide. The microorganism conversion method has a very high catalytic efficiency, increases the substrate conversion rate, under a material concentration of 3.5 mol / L, the 2,6-difluorobentrinile conversion rate is as high as 100%, the 2,6-difluorobenamide selectivity is 100%, and no by product 2,6- difluorobenzoic acid is generated. The separation and purification technology of target product is simplified, and the method has the advantages of mild reaction conditions, low requirements on equipment, and easy application to production.

Description

technical field [0001] The invention belongs to the field of biotechnology, in particular to a method for preparing 2,6-difluorobenzamide by using Rhodococcus rubrum. Background technique [0002] The appearance of 2,6-difluorobenzamide is white needle-like crystalline powder. It is a key intermediate in the synthesis of benzoylurea insecticides. Synthesis of substances to block the growth, development and reproduction of insects. Its insecticidal mechanism is unique, efficient, broad-spectrum, low-toxic, safe for humans and animals, and has no cross-resistance with other insecticides. It is an environmentally friendly insecticide. New varieties of agents. In the past ten years, benzoylurea pesticides have been developed rapidly in the world, and diflubenzuron, hexaflumuron, flubenzuron, diflubenuron, flubenzuron, diflubenuron, diflubenuron, and flufenuron have been developed. And other products, and 2,6-difluorobenzamide is the key intermediate for the synthesis of these ...

Claims

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Application Information

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IPC IPC(8): C12P13/02C12R1/01
Inventor 王敏申雁冰翟莹郑宇
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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