Crystallization method of iprodione

A technology of crystallization of iprodione, which is applied in the field of crystallization of iprodione, can solve problems such as low purity, high cost, and environmental protection, and achieve the effects of improving purity, improving crystal form, and improving stability

Active Publication Date: 2022-04-15
XINYI AGRI CHEM PLANT JIANGSU PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Therefore, the technical problem to be solved by the present invention is to overcome the defects of the existing iprodione crystallization by the toluene-n-hexane method that the purity is not high, it is not environmentally friendly, and the cost is high, so as to provide a kind of iprodione with high purity, less pollution and low cost. Bacteriozuron crystallization method

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  • Crystallization method of iprodione

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Embodiment 1

[0031] The present embodiment provides a crystallization method of iprodione, comprising the following steps:

[0032] Step (A), the preparation of iprodione

[0033] Feeding coefficient: toluene 400ml, hydantoin 85g, isopropyl isopropyl ester 40g, triethylamine 14g, catalyst 0.6g, condensation reaction occurs after mixing, pickling and water washing, and organic urea dissolved in iprodione is collected. Mutually.

[0034] Step (B), crystallization of iprodione

[0035] The toluene organic phase dissolved with iprodione was transferred to a 1000ml flask, and the organic solvent toluene was removed by a vacuum evaporator under negative pressure. When there is solid precipitation on the inner wall of the flask, about 280ml of toluene is removed at this time, and the acetic acid aqueous solution with pH=5 is started dropwise, and the toluene is removed under negative pressure while dropping. Control the dripping speed of acetic acid aqueous solution so that the dripping speed ...

Embodiment 2

[0038] The present embodiment provides a crystallization method of iprodione, comprising the following steps:

[0039] Step (A), the preparation of iprodione

[0040] Feeding coefficient: toluene 400ml, hydantoin 85g, isopropyl isopropyl ester 40g, triethylamine 14g, catalyst 0.6g, condensation reaction occurs after mixing, pickling and water washing, and organic urea dissolved in iprodione is collected. Mutually.

[0041] Step (B), crystallization of iprodione

[0042] The toluene organic phase dissolved with iprodione was transferred to a 1000ml flask, and the organic solvent toluene was removed by a vacuum evaporator under negative pressure. When there is solid precipitation on the inner wall of the flask, about 280ml of toluene is removed at this time, and the acetic acid aqueous solution with pH=6 is started dropwise, and the toluene is removed under negative pressure while dropping. Control the speed of acetic acid aqueous solution dripping, make the dropping speed of...

Embodiment 3

[0045] The present embodiment provides a crystallization method of iprodione, comprising the following steps:

[0046] Step (A), the preparation of iprodione

[0047] Feeding coefficient: toluene 400ml, hydantoin 85g, isopropyl isopropyl ester 40g, triethylamine 14g, catalyst 0.6g, condensation reaction occurs after mixing, pickling and water washing, and organic urea dissolved in iprodione is collected. Mutually.

[0048] Step (B), crystallization of iprodione

[0049] The toluene organic phase dissolved with iprodione was transferred to a 1000ml flask, and the organic solvent toluene was removed by a vacuum evaporator under negative pressure. When there is solid precipitation on the inner wall of the flask, remove about 280ml of toluene at this time, start to drop the acetic acid aqueous solution with pH=5.5, and continue to remove toluene under negative pressure while dropping, during this process, according to the speed of toluene removal To control the speed of the aqueo...

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Abstract

The invention belongs to the technical field of pesticide synthesis, and in particular relates to a crystallization method of iprodione. In the crystallization method of iprodione provided by the present invention, the organic phase in which iprodione is dissolved is removed from the organic solvent under negative pressure. Reflux in the solvent system to dissolve the clear, and then remove the weak acid aqueous solution and residual organic solvents, avoiding the problem of heterogeneous nucleation of iprodione in the crystallization process, reducing the coating amount of impurities inside the crystal, and improving the purity; Crystal form, high crystal packing density, which improves the stability of the product; avoids the use of conventional n-hexane, and improves the operating environment.

Description

technical field [0001] The invention belongs to the technical field of pesticide synthesis, and in particular relates to a crystallization method of iprodione. Background technique [0002] Iprodione, the common name in English is Iprodione, and its aliases are prodihydrin, 3-(3,5-dichlorophenyl)-1-isopropylcarbamoylhydantoin. Iprodione is poorly soluble in water, easily soluble in acetone, dimethylformamide and other organic solvents, decomposed in case of alkali, non-hygroscopic and non-corrosive. As a dicarboximide high-efficiency broad-spectrum, contact-type fungicide, iprodione is suitable for the prevention and treatment of early leaf defoliation, gray mold, early blight and other diseases of various fruit trees, vegetables, melons and other crops. [0003] At present, the synthesis method of iprodione on the market is mainly divided into four steps. 3,5-dichloroaniline is used as raw material, and phosgene is reacted with phosgene to generate 3,5-dichlorophenylisocya...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/80
CPCC07D233/80C07B2200/13
Inventor 顾思雨张贤振蒋磊周全义许思如
Owner XINYI AGRI CHEM PLANT JIANGSU PROV
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