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Synthesis method of high-purity butralin

A synthesis method and high-purity technology, applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems of low purity of butadiene, and achieve the effect of simple synthesis method and improved purity

Inactive Publication Date: 2013-07-24
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The purpose of the present invention is to solve the problem that the existing synthetic method obtains the low purity of butaline, and provides a kind of synthetic method of high-purity butaline

Method used

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  • Synthesis method of high-purity butralin
  • Synthesis method of high-purity butralin
  • Synthesis method of high-purity butralin

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Experimental program
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Effect test

specific Embodiment approach 1

[0021] Specific embodiment one: the synthetic method of the high-purity Zhongbutaline of the present embodiment realizes according to the following steps:

[0022] 1. Add 295-305g of dichloroethane and 35-40g of p-tert-butylphenol into a four-necked flask equipped with a condenser, heat to 45-55°C, then add 45-50g of nitric acid solution dropwise, and react for 12- For 18 minutes, continue to heat up to 68-72°C, then transfer to a separatory funnel, let stand to separate the upper layer of acid water to obtain the mononitrated organic phase, and then transfer the mononitrated organic phase to a four-necked flask equipped with a condenser. Heat to 45-55°C, add 22-26g of concentrated nitric acid dropwise, react for 12-18 minutes, continue to heat up to 68-72°C, then transfer to a separatory funnel, let stand to separate the upper layer of acid water, and obtain the dinitrated organic phase , transfer the dinitrated organic phase into a four-necked bottle with a condensation wate...

specific Embodiment approach 2

[0033] Specific embodiment 2: The difference between this embodiment and specific embodiment 1 is that the time used for adding 48.6 g of nitric acid solution dropwise in step 1 is 45 minutes. Other steps and parameters are the same as those in Embodiment 1.

specific Embodiment approach 3

[0034] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is that step one takes 30 minutes to add 24.3 g of concentrated nitric acid dropwise. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

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Abstract

The invention provides a synthesis method of high-purity butralin, relates to a synthesis method of butralin, and solves the problem of the conventional synthesis method that the obtained butralin has relatively low purity. The synthesis method comprises the following steps of: 1, heating and mixing dichloroethane with p-tert-butylphenol; dropping salpeter solution; dropping concentrated nitric acid to carry out a nitratlon reaction after the upper acid water is separated; adding water; heating and refluxing; cooling through an ice-water bath; and then carrying out extraction filtration and recrystallization to obtain a nitration product; 2, adding 2-butanone, potassium iodide and potassium carbonate to the nitration product; heating; dropping dimethyl sulfate; heating to evaporate the 2-butanone; adding water to reflux; and then filtering and recrystallizing to obtain a methylate; and 3, heating and mixing the methylate with methanol; dropping sec-butylamine to react for a time; adding water; heating; and then filtering to obtain the high-purity butralin. The purity of the butralin obtained through the synthesis method is up to more than 99%; and the synthesis method is mainly applied to the synthesis of the butralin.

Description

technical field [0001] The invention relates to a method for synthesizing secbutaline. Background technique [0002] Zhong Dingling, Chinese alias: Diloamine, English name: Butralin; Dibutaline, also known as bud-stopping element, is contact killing and local systemic bud suppressant, belongs to the dinitroaniline tobacco bud suppressant of low toxicity, has a good effect on The growth inhibition effect of axillary buds is high, and the drug effect is fast. Its structural formula is: [0003] [0004] Zhongbuling is a herbicide for selective pre-emergent soil treatment. Its effect is similar to that of trifluralin. After the agent enters the plant, it mainly inhibits the cell division of the meristem, thereby inhibiting the growth of weed buds and young roots. It can also be used as a plant growth regulator to control the growth of tobacco axillary buds. It is mainly suitable for controlling barnyard grass, goosegrass, crabgrass, foxtail and other annual monocotyledono...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/52C07C209/18
Inventor 温彦鹏姚林山高金胜白有银
Owner HEILONGJIANG UNIV
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