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Method for preparing bromoxynil octanoate

A technology for octanoyl bromoxynil and bromoxynil, which is applied in the field of octanoyl bromoxynil synthesis, can solve the problems of high price of octanoyl chloride, environmental pollution and high reaction temperature, and achieves enhanced mass transfer effect, shortened reaction time, and reduced reaction time. fast effect

Pending Publication Date: 2022-06-03
NANJING ADVANCED BIOLOGICAL MATERIALS & PROCESS EQUIP INST CO LTD +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the existing literature 1 (Cao Genfa, Yang Jianping, Miao Weifang. Synthesis of octanoyl bromoxynil [J]. Zhejiang Chemical Industry, 2001, (2): 48-49.), there are many waste waters, serious environmental pollution, and The high price of octanoyl chloride leads to complex production process and high production cost
[0004] In existing literature 2 (Liu Yuan, Liao Daohua. Direct synthesis of bromoxynil octanoate [J]. Fine Chemical Industry, 2002, (4): 193-194.) by octanoic acid, poisonous dimethylformamide (DMF ) as a solvent, polluting the environment
[0005] In the existing literature 3 (Xu Yao, Qian Shengle, Chen Fan. Improvement of the synthesis process of bromoxynil octanoyl[J]. Journal of Wenzhou University, 2008,29(6):17-20.), the reaction temperature is high and the time long, complicated

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  • Method for preparing bromoxynil octanoate
  • Method for preparing bromoxynil octanoate
  • Method for preparing bromoxynil octanoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042]Take 48g (0.4mol) of 4-hydroxybenzonitrile, add 480g of absolute ethanol and mix to obtain a homogeneous organic solution; take 297g (1.76mol) of 48% aqueous hydrobromic acid solution; take 100g (0.88mol) of 30% peroxide oxidation Hydrogen aqueous solution; pour the prepared three materials into the corresponding raw material tanks respectively, set the temperature of the microreactor 1 to 5 °C, open the ultrasonic-assisted (frequency 35Hz) microreactor 2, and set the temperature of the ultrasonic device to 50 °C. °C. The hydrobromic acid aqueous solution and the hydrogen peroxide aqueous solution were pumped into the microreactor 1, wherein the hydrobromic acid aqueous solution was pumped in at a flow rate of 4 mL / min, and the hydrogen peroxide aqueous solution was pumped in at a flow rate of 1.8 mL / min. The reaction temperature was 5°C, and the reaction residence time was 5 min to obtain an aqueous solution of bromine. The 4-hydroxybenzonitrile solution and the bromin...

Embodiment 2

[0043] Example 2: Comparative Example 1, hydrobromic acid reduced by 25%.

[0044] Take 48g (0.4mol) of 4-hydroxybenzonitrile, add 480g of absolute ethanol and mix to obtain a homogeneous organic solution; take 223g (1.32mol) of 48% aqueous hydrobromic acid solution; take 100g (0.88mol) of 30% peroxide oxidation Hydrogen aqueous solution; pour the prepared three materials into the corresponding raw material tanks respectively, set the temperature of the microreactor 1 to 5 °C, open the ultrasonic-assisted (frequency 35Hz) microreactor 2, and set the temperature of the ultrasonic device to 50 °C. °C. The hydrobromic acid aqueous solution and the hydrogen peroxide aqueous solution were pumped into the microreactor 1, wherein the hydrobromic acid aqueous solution was pumped in at a flow rate of 4 mL / min, and the hydrogen peroxide aqueous solution was pumped in at a flow rate of 1.8 mL / min. The reaction temperature was 5°C, and the reaction residence time was 5 min to obtain an a...

Embodiment 3

[0045] Example 3: Comparative Example 1, without ultrasonic assistance

[0046] Take 50.88g (0.424mol) of 4-hydroxybenzonitrile, add 508g of absolute ethanol and mix to obtain a homogeneous organic solution; take 315g (1.87mol) of 48% aqueous hydrobromic acid; take 106g (0.93mol) of 30% peroxide Hydrogen oxide aqueous solution; pour the prepared three materials into the corresponding raw material tanks respectively, set the temperature of the microreactor 1 to 5°C, open the ultrasonic-assisted (frequency 35Hz) microreactor 2, and set the temperature of the ultrasonic device to 50°C. The hydrobromic acid aqueous solution and the hydrogen peroxide aqueous solution were pumped into the microreactor 1, wherein the hydrobromic acid aqueous solution was pumped in at a flow rate of 4 mL / min, and the hydrogen peroxide aqueous solution was pumped in at a flow rate of 1.8 mL / min. The reaction temperature was 5°C, and the reaction residence time was 5 min to obtain an aqueous solution o...

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Abstract

The invention discloses a method for preparing bromoxynil octanoate, which comprises the following steps: in a microchannel reaction device, reacting hydrogen peroxide water with hydrobromic acid to obtain bromine, and then reacting bromine with 4-hydroxybenzonitrile to obtain a bromoxynil crude product; in another micro-channel reaction device, the n-octanoic acid and thionyl chloride react to obtain capryloyl chloride, and then the capryloyl chloride and bromoxynil react to obtain the final product bromoxynil octanoate. Compared with the traditional preparation method of bromoxynil octanoate, the method disclosed by the invention has the advantages of two-step continuity, short reaction time, low cost, high yield, few byproducts, simplicity in operation, small amplification effect, high safety and suitability for industrial production.

Description

technical field [0001] The invention belongs to the technical field of octanoyl bromoxynil synthesis, in particular to a method for preparing octanoyl bromoxynil. Background technique [0002] Octanoyl bromoxynil is a very stable herbicide and is therefore widely used. Most of the traditional preparation methods are kettle-type reactions, which have problems such as high cost, long reaction time, high reaction temperature, serious environmental pollution of waste water, complex production process and certain difficulties in industrial production. E.g: [0003] In the existing literature 1 (Cao Genfa, Yang Jianping, Miao Weifang. Synthesis of octanoyl bromoxynil [J]. Zhejiang Chemical Industry, 2001, (2): 48-49.), the waste water produced is more, the environmental pollution is serious, and The high price of octanoyl chloride leads to complicated production process and high production cost. [0004] In existing literature 2 (Liu Yuan, Liao Daohua. Direct synthesis of bromo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/53C07C255/55B01J19/00
CPCC07C253/30B01J19/0093C07C255/53C07C255/55
Inventor 陆帅乔凯黄达赵跃李玉光郭凯
Owner NANJING ADVANCED BIOLOGICAL MATERIALS & PROCESS EQUIP INST CO LTD
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