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Method for improving anti-caking property of tebuconazole

A technology of tebuconazole and anti-caking, applied in the direction of organic chemistry, etc., can solve the problems of poor anti-caking

Active Publication Date: 2014-07-16
北京颖泰嘉和分析技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the problem of poor caking resistance of existing tebuconazole products and provide a method for improving the caking resistance of tebuconazole

Method used

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  • Method for improving anti-caking property of tebuconazole

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0026] Preparation Example 1: 120 grams of 1-(4-chlorophenethyl)-1-tert-butyl-1,2-oxirane, 3 grams of potassium hydroxide, 40 grams of 1,2,4,-triazole, Add 1 g of N,N-dimethyl-4-aminopyridine and 100 ml of n-butanol into a 500 ml three-neck flask with a stirring and reflux tube, and stir for 6 hours at a reflux temperature of 120°C. After the reaction is complete, add hydrochloric acid to neutralize, The phases were separated, the organic phase was cooled and crystallized, washed with water, filtered and dried to obtain 102 g of a white solid with a purity of ≥98% by weight and a particle size of D90=188.60 μm. Poor caking resistance.

preparation example 2

[0027] Preparation example 2: 120 grams of 1-(4-chlorophenethyl)-1-tert-butyl-1,2-oxirane, 6 grams of potassium hydroxide, 40 grams of 1,2,4,-triazole, Add 1 g of N,N-dimethylaniline and 100 ml of dimethylformamide into a 500 ml three-necked flask with a stirring and reflux tube, and stir for 4 hours at a reflux temperature of 130 ° C. After the reaction is complete, add hydrochloric acid for neutralization and negative pressure The solvent was recovered by distillation, the organic phase was cooled and crystallized, washed with water, filtered and dried to obtain 106 g of a white solid with a purity of ≥98.6% by weight and a particle size of D90=180.85 μm. Poor caking resistance.

preparation example 3

[0028] Preparation Example 3: 120 grams of 1-(4-chlorophenethyl)-1-tert-butyl-1,2-oxirane, 7 grams of sodium ethoxide, 40 grams of 1,2,4,-triazole, 0.5 Add 1 g of N,N-dimethyl-4-aminopyridine and 100 ml of n-butanol into a 500 ml three-neck flask with a stirring and reflux tube, and stir for 6 hours at a reflux temperature of 120 ° C. After the reaction is complete, add hydrochloric acid to neutralize and negatively The solvent was recovered by distillation under pressure, the organic phase was cooled and crystallized, filtered and dried to obtain 101 grams of white solid, the purity was ≥98.3% by weight, and the particle size D90=192.47 microns. Poor caking resistance.

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Abstract

The invention discloses a method for improving anti-caking property of tebuconazole, wherein the method comprises the following steps: dissolving tebuconazole in an organic solvent, thereby obtaining a tebuconazole solution, and then cooling and crystallizing the tebuconazole solution, wherein the particle size of the obtained crystal is D90 from 250 to 305 microns due to the cooling and crystallizing condition. The caking problem during transportation and storage processes is effectively overcome by the tebuconazole product obtained according to the method provided by the invention.

Description

technical field [0001] The invention relates to a method for improving the caking resistance of tebuconazole. Background technique [0002] Tebuconazole ((RS)-1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol ), is a low-toxic and high-efficiency triazole fungicide developed by Bayer Corporation of Germany with systemic, protective, therapeutic and eradicating activities. It is a sterol demethylation inhibitor and is used for seed treatment or foliar spraying of important economic crops. Its structure is: [0003] [0004] CN200510032349 discloses a method for preparing high-purity tebuconazole. In the method, a catalyst is added to the chemical reaction of synthesizing tebuconazole to synthesize a high-purity and high-yield tebuconazole powder product with a product purity of ≥98% by weight. The yield is ≥80% by weight, and the particle size is generally D90 less than 200 microns. However, during the storage and transportation of the tebuconaz...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/08
Inventor 谭徐林罗进超王春艳邢文龙李咏静倪肖元
Owner 北京颖泰嘉和分析技术有限公司
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