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Preparation process for bromoxynil octanoate

A technology for the preparation of bromoxynil octanoyl, which is applied in the field of bromoxynil octanoyl preparation, can solve the problems of low degree of production automation, the need to recycle bromine mother liquor, and environmental pollution accidents, so as to reduce the incidence of pollution accidents , reduce production costs, and avoid the effect of dry powder feeding

Inactive Publication Date: 2015-09-23
JIANGSU HEBEN BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the bromoxynil produced by bromination is a solid, it needs to be separated by centrifugation, and the transfer requirements after centrifugation are extremely high. Once leaked, it will cause serious environmental pollution accidents
Moreover, the bromine mother liquor needs to be recovered, the labor intensity is high, and the degree of production automation is low.

Method used

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  • Preparation process for bromoxynil octanoate
  • Preparation process for bromoxynil octanoate
  • Preparation process for bromoxynil octanoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 250ml four-necked bottle, add 23.8g (0.2mol) of p-hydroxybenzonitrile and 33.2g (0.204mol) of octanoyl chloride, raise the temperature to 105±5°C, keep it warm for 3 hours, take a sample, and after the reaction is qualified, evaporate the excess octanoyl chloride. acid chloride. After steaming octanoyl chloride, cool down to 50±5°C, add 120ml of dichloroethane and 0.5g of tetra-n-butylammonium bromide, control the temperature at 50±5°C, add dropwise 27.2g (0.4mol) of 50% hydrogen peroxide and 32g (0.2mol) of bromine, dropwise for about 4 hours, after the dropwise addition is completed, keep warm for 30 minutes, take a sample for testing, after the reaction is qualified, add a small amount of alkali to destroy the hydrogen peroxide, use starch potassium iodide test paper to pass the test, heat up to remove the solvent, When the temperature rises to 95°C, stop the distillation, add 100ml of process water, keep warm at 90°C for 30 minutes, pour it into a separatory fu...

Embodiment 2

[0020] In a 250ml four-necked bottle, add 23.8g (0.2mol) p-hydroxybenzonitrile and 33.2g (0.204mol) octanoyl chloride, raise the temperature to 105±5°C, keep it warm for 3 hours, take a sample, after the reaction is qualified, evaporate the excess octanoyl chloride. After steaming octanoyl chloride, cool down to 50±5°C, add 120ml cyclohexane and 0.5g tetra-n-butylammonium bromide, control the temperature at 50±5°C, add dropwise 27.2g (0.4mol) 50% hydrogen peroxide and 32g (0.2mol) bromine, about 4 hours of dripping time, after the dropwise addition, keep warm for 30 minutes, take a sample and detect, after the reaction is qualified, add a small amount of alkali, destroy hydrogen peroxide, pass the test with starch potassium iodide test paper, heat up and remove the solvent, wait The temperature rises to 95°C, stop the distillation, add 100ml of process water, keep warm at 90°C for 30 minutes, pour it into a separatory funnel, wash the lower organic phase with water, separate t...

Embodiment 3

[0022] In a 250ml four-necked bottle, add 23.8g (0.2mol) p-hydroxybenzonitrile and 33.2g (0.204mol) octanoyl chloride, raise the temperature to 105±5°C, keep it warm for 3 hours, take a sample, after the reaction is qualified, evaporate the excess octanoyl chloride. After steaming octanoyl chloride, cool down to 50±5°C, add 120ml of methanol and 0.5g of tetra-n-butylammonium bromide, control the temperature at 50±5°C, add dropwise 27.2g (0.4mol) of 50% hydrogen peroxide and 32g (0.2 mol) bromine, the dropping time is about 4 hours, after the dropping is completed, keep warm for 30 minutes, take a sample test, after the reaction is qualified, add a small amount of alkali, destroy the hydrogen peroxide, use the starch potassium iodide test paper to test qualified, heat up to remove the solvent, wait for the temperature to rise To 95°C, stop the distillation, add 100ml of process water, keep warm at 90°C for 30 minutes, pour it into a separatory funnel, wash the lower organic pha...

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Abstract

The invention discloses a preparation process for bromoxynil octanoate. The preparation process is characterized in that octanoyl chloride, 4-cyanophenol, 50% hydrogen peroxide and bromine are used as reaction raw materials and the preparation process comprises an esterification reaction step and a bromination reaction step according to a reaction sequence. The preparation process has the advantages as follows: the steps of bromination mother liquor recovery, centrifugation and drying are eliminated, dry powder feeding is avoided, the occurrence rate of contamination accidents is reduced, the yield is increased, material consumption is reduced, equipment investment is reduced and the production cost is reduced.

Description

technical field [0001] The invention relates to a preparation process of bromoxynil octanoyl, which belongs to the technical field of synthesis of pesticide raw materials. Background technique [0002] Bromoxynil octanoyl, also known as bromoxynil octanoate, is a benzonitrile contact herbicide with certain systemic activity. In 1963, the first benzonitrile contact herbicide bromoxynil was developed by Bayer Company of Germany. Because of its strong stability of octanoyl ester, bromoxynil is mostly used in practical applications. [0003] Bromoxynil octanoyl is a contact-killing herbicide for selective post-emergence stem and leaf treatment. It is mainly absorbed by leaves and has a very limited conduction in plants. It inhibits various processes of photosynthesis, including photophosphorylation and electron transfer. In particular, the Hill reaction of photosynthesis causes rapid necrosis of plant tissues, thereby achieving the purpose of herbicide. [0004] At present, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/55C07C253/30
Inventor 葛中群张兵陈张唯
Owner JIANGSU HEBEN BIOCHEM
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