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A kind of preparation method of three (2,4-dichloro-5-nitrophenyl) phosphate

A technology of nitrophenyl and dichlorophenyl, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of environmental pollution and low yield of waste mixed acids, To achieve the effect of effective selectivity, lower production cost and reasonable synthesis process

Active Publication Date: 2018-01-16
LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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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 waste mixed acid polluting the environment and low yield in the preparation of tris(2,4-dichloro-5-nitrophenyl) phosphate by mixed acid nitration in the prior art oxadiazone production process, the present invention provides a The preparation method of tris(2,4-dichloro-5-nitrophenyl) phosphate which is environment-friendly, low in cost and high in yield provides raw materials for the production of oxadiazone and further satisfies the market demand for oxadiazone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 1000mL four-neck round bottom flask equipped with mechanical stirring, thermometer and condenser, add 120g of chloroform, 53.5g of tris(2,4-dichlorophenyl) phosphate, 3g of activated carbon and 1.02g of catalyst Acetic anhydride, stirring down to below 5°C, start dropwise adding 29.08g of 65% nitric acid, control the temperature at 5-10°C, after the addition, gradually raise the temperature to 10-20°C, react for 2 hours, and then raise the temperature to 30-20°C React at 40°C for 3 hours. After the reaction, cool down to room temperature, filter to remove the carrier compound, separate the organic phase, and remove the solvent to obtain 57.5g of tris(2,4-dichloro-5-nitrophenyl) Phosphate ester, content 98.3%, yield 97.8%.

Embodiment 2

[0030] In a 1000mL four-neck round bottom flask equipped with mechanical stirring, thermometer and condenser, add 300g of chloroform, 53.5g of tris(2,4-dichlorophenyl) phosphate, 3g of activated carbon and 2.55g of catalyst Acetic anhydride, stir to drop below 5°C, start to drop 29.65g of 85% nitric acid, control the temperature at 5-10°C, after the dropwise addition, gradually raise the temperature to 10-20°C, react for 3 hours, and then raise the temperature to 30-20°C React at 40°C for 4 hours. After the reaction, cool down to room temperature, filter to remove the carrier compound, separate the organic phase, and remove the solvent to obtain 57.6g of tris(2,4-dichloro-5-nitrophenyl) Phosphate ester, content 98.4%, yield 98.1%.

Embodiment 3

[0032] In a 1000mL four-neck round bottom flask equipped with mechanical stirring, thermometer and condenser, add 600g of chloroform, 53.5g of tris(2,4-dichlorophenyl) phosphate, 3g of activated carbon and 5.1g of catalyst Acetic anhydride, stir to drop below 5°C, start to add 33.16g of 95% nitric acid dropwise, control the temperature at 5-10°C, after the dropwise addition, gradually raise the temperature to 10-20°C, react for 5 hours, and then raise the temperature to 30-30°C React at 40°C for 6 hours. After the reaction, cool down to room temperature, filter to remove the carrier compound, separate the organic phase, and remove the solvent to obtain 57.8g of tris(2,4-dichloro-5-nitrophenyl) Phosphate ester, content 98.5%, yield 98.6%.

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Abstract

The invention discloses a method for preparing tris (2,4-dichloro-5-nitrophenyl) phosphate. First, dissolving tris (2,4-dichlorophenyl) phosphate, a carboxylic acid anhydride catalyst and a carrier material in chlorinated paraffins, mixing by stirring, cooling down to below 5 DEG C, dropwise adding concentrated nitric acid solution, and controlling the temperature at 5-10 DEG C; after the dropwise addition raising the temperature to 10-20 DEG C and reacting for 2-6 h; then heating to 30-60 DEG C, reacting for 3-10 h; and after the reaction, cooling to room temperature, filtering, layering an organic phase, and removing the solvent to obtain the tris (2,4-dichloro-5-nitrophenyl) phosphate. According to the invention, tris (2,4-dichlorophenyl) phosphate and nitric acid are reacted in a solvent of chlorinated paraffins in the presence of carboxylic acid anhydride, so as to fundamentally avoid the environment pollution caused by waste mixed acid produced by the conventional acid nitration process; at the same time, the method has the advantages of more effective selectivity of the nitration reaction, significantly increased yield of the tris(2,4-dichloro-5-nitrophenyl) phosphate, reduction of production costs and reduction of environmental pollution, and has broad application prospects in oxadiazon industrial production.

Description

technical field [0001] The invention relates to the preparation of an intermediate tris(2,4-dichloro-5-nitrophenyl)phosphate of a protoporphyrinogen oxidase inhibitor selective pre-emergence and post-emergence herbicide variety oxadiazon method, belonging to the field of organic chemistry. Background technique [0002] Oxadiazon is a protoporphyrinogen oxidase inhibitor selective pre-emergence and post-emergence herbicide variety. It was discovered in 1963 that it has significant herbicidal activity and is suitable for rice, cotton, soybean, sugarcane, sunflower, peanut and A variety of tuber crops or transplanted crops can be applied before or after emergence, mainly to control gramineous and broad-leaved weeds. Now oxadiazone has been registered in Brazil, Bulgaria, Colombia, Ecuador, Spain, Iran, Italy, Japan, Mexico, Peru, Romania, Senegal and other countries for use in rice fields, and in France, West Germany, Spain and Austria for use in vineyards and orchard weeding...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/12
CPCC07F9/12
Inventor 石卫兵戴翠红房雷
Owner LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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