A kind of preparation method of 2,4-dichloro-5-nitrophenol
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A technology of nitrophenol and nitrophenyl, which is applied in the field of organic chemistry, can solve the problems of low yield and pollution of the environment by waste acid, and achieve the effects of reducing production costs, reasonable synthesis process, and avoiding pollution
Active Publication Date: 2017-09-22
LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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[0008] In order to solve the problem of serious environmental pollution and low yield of waste acid produced in the existing synthesis process of 2,4-dichloro-5-nitrophenol, the present invention provides an environmentally friendly, low-cost, high-yield 2 , the preparation method of 4-dichloro-5-nitrophenol
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Embodiment 1
[0027] In a 1000mL four-neck round bottom flask equipped with mechanical stirring, thermometer and condenser tube, add 96g methanol, 57.8g tris(2,4-dichloro-5-nitrophenyl) phosphate and 0.586g catalyst tri Lanthanum fluoromethanesulfonate, 0.72g tetrahydrofuran, stirred and gradually raised to reflux temperature, reacted for 3h, after the reaction was completed, the catalyst was separated by filtration, and after the solvent was removed, 62.7g of 2,4-dichloro-5-nitrophenol was obtained , content 98.0%, yield 98.5%.
Embodiment 2
[0029] In a 1000mL four-neck round bottom flask equipped with mechanical stirring, thermometer and condenser tube, add 192g methanol, 57.8g tris(2,4-dichloro-5-nitrophenyl) phosphate and 2.93g catalyst tri Lanthanum fluoromethanesulfonate, 1.8g tetrahydrofuran, stirred and gradually heated to reflux temperature, reacted for 5h, after the reaction was completed, the catalyst was separated by filtration, and after the solvent was removed, 62.8g of 2,4-dichloro-5-nitrophenol was obtained , content 98.3%, yield 99.0%.
Embodiment 3
[0031] In a 1000mL four-neck round bottom flask equipped with mechanical stirring, thermometer and condenser tube, add 288g methanol, 57.8g tris(2,4-dichloro-5-nitrophenyl) phosphate and 5.86g catalyst tri Lanthanum fluoromethanesulfonate, 3.6g tetrahydrofuran, stirred and gradually heated to reflux temperature, reacted for 7 hours, after the reaction was completed, the catalyst was separated by filtration, and after the solvent was removed, 63.2g of 2,4-dichloro-5-nitrophenol was obtained , content 98.5%, yield 99.8%.
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Abstract
The invention discloses a method for preparing 2,4-dichloro-5-nitrophenol. The method is as below: first, evenly mixing tris(2,4-dichloro-5-nitrophenyl) phosphate, rare earth trifluoromethyl sulfonate catalyst, a cocatalyst and an alcoholic solvent; then gradually heating to a reflux temperature, reacting for more than 3h; and cooling to room temperature after the reaction, separating the catalyst by filtration, and removing the solvent in a liquid phase by distillation to obtain the 2,4-dichloro-5-nitrophenol. In the presence of the co-catalyst, tris (2,4-dichloro-5-nitrophenyl) phosphate reacts with the alcohol solvent under the catalysis of rare earth trifluoromethyl sulfonate, so as to fundamentally avoid the environmental pollution caused by the large quantities of waste acid in the traditional hydrolysis; the reaction is more thorough; and the method increases the yield of the product 2,4-dichloro-5-nitrophenol from 88% to 98%, increases the purity from 91.5 % to 97.5%, lowers production costs, and plays a positive role for the industrial development of oxadiazon.
Description
technical field [0001] The invention relates to a preparation method of an intermediate 2,4-dichloro-5-nitrophenol of a protoporphyrinogen oxidase inhibitor selective pre-emergence and post-emergence herbicide variety oxadiazon, 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. After that, it has been tested in laboratories, greenhouses and fields all over the world. A large number of tests have proved that its efficacy is good. Oxadiazone is suitable for rice, cotton, soybean, sugarcane, sunflower, peanut and various tuber crops or transplanted crops. It can be applied before or after emergence to control grass and broad-leaved weeds. It is now registered for use in rice fields in Brazil, Bulgaria, Colombia, Ecuador, Spain, Iran, Italy, Japan, Mexico, Peru, Romania...
Claims
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