Method to separate enriched Z and E types of 3-chloro-2-(4-fluorophenyl)-1-(2-chlorophenyl)propylene

A technology of separation and enrichment, fluorophenyl, applied in organic chemistry methods, halogenated hydrocarbon disproportionation separation/purification, organic chemistry, etc., can solve the problems of inability to produce high purity, unstable performance, low technical level, etc. Stability of product quality and yield, shortened production and processing cycles, and high product purity

Inactive Publication Date: 2018-09-14
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above-mentioned methods all have low technical level, cannot produce high-purity (Z)-3-chloro-2-(4-fluorophenyl)-1-(2-chlorophenyl)propene, and the production cost is high, and

Method used

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  • Method to separate enriched Z and E types of 3-chloro-2-(4-fluorophenyl)-1-(2-chlorophenyl)propylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Rotate the mixed solution rich in Z-type and E-type 3-chloro-2-(4-fluorophenyl)-1-(2-chlorophenyl)propene at 50°C and 80°C respectively to remove methanol and Toluene;

[0026] 2. Take four clean and dry beakers (number: hexane 1, hexane 2, hexane 3, hexane 4), add 15mL of hexane into each beaker, then add 2mL, 5mL, 10mL and 15mL of the above-mentioned rotary evaporation liquid was obtained to obtain the first solution;

[0027] 3. Freeze the solution in a -80°C refrigerator;

[0028] 4. After about 4-6 hours, stratification occurs, and the upper layer is a colorless transparent liquid. The upper liquid is separated at low temperature to obtain the second solution, which is sampled for HPLC. The numbers are hexane 1-up, hexane 2-up, hexane Alkane 3-on, hexane 4-on;

[0029] 5. The lower layer is a dark brown solid. Place it in a refrigerator at -30°C. After about 6 minutes, it will melt, and the third solution will be obtained. Samples will be tested for HPLC. -X...

Embodiment 2

[0035] 1. Rotate the mixed solution rich in Z-type and E-type 3-chloro-2-(4-fluorophenyl)-1-(2-chlorophenyl)propene at 50°C and 80°C respectively to remove methanol and Toluene;

[0036] 2. Take four clean and dry beakers (number: n-pentane 1, n-pentane 2, n-pentane 3, n-pentane 4), add 15mL of n-pentane to each beaker, and then add 2mL dropwise , 5mL, 10mL and 15mL of the above rotary evaporation liquid to obtain the first solution;

[0037] 3. Freeze the solution in a -80°C refrigerator;

[0038] 4. After about 4-6 hours, stratification occurs. The upper layer is a colorless transparent liquid. The upper liquid is separated at low temperature to obtain the second solution, which is sampled for HPLC. The numbers are n-pentane 1-up and n-pentane 2-up respectively. , n-pentane 3-up, n-pentane 4-up;

[0039] 5. The lower layer is a dark brown solid, placed in a refrigerator at -30°C, it will melt after about 2 minutes, and the third solution is obtained, and samples are taken...

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Abstract

The invention discloses a method to separate enriched Z and E types of 3-chloro-2-(4-fluorophenyl)-1-(2-chlorophenyl)propylene, comprising the steps of (1) mixing a mixed solution, having rich Z and Etypes of 3-chloro-2-(4-fluorophenyl)-1-(2-chlorophenyl)propylene with an organic solvent in a volume ratio of 1:(1-7.5) such that the mixed solution is fully dissolved in the organic solvent to obtain a first solution; (2) freezing a container with the first solution at the low temperature of -70 DEG C to -90 DEG C; (3) after the solution of step (2) layers, separating to obtain supernate so thatE-type solution is obtained; (4) after material left after the separation of step (3) is frozen into solid, thawing the solid at the temperature of -20 DEG C to -30 DEG C; (5) after the solid of step(4) thaws, and collecting thawed liquid that is Z-type solution. The method herein is a purely-mechanical freeze-separation method; the product obtained has high purity, free of nature change, good in performance stability, and higher in quality and yield stability.

Description

technical field [0001] The invention belongs to the technical field of epoxiconazole production, in particular to a method for separating and enriching Z-type and E-type 3-chloro-2-(4-fluorophenyl)-1-(2-chlorophenyl)propene. Background technique [0002] Epoxiconazole (Epoxiconazole) trade name Oubo, is a new, broad-spectrum, long-lasting triazole fungicide, developed by BASF in 1983. This product is a triazole fungicide, which has a good control effect on a series of cereal crops such as blight, powdery mildew, eye striae and more than ten kinds of diseases, and can control sugar beet, peanut, rape, lawn, Diseases of coffee, rice and fruit trees; not only has good protection, treatment and eradication activities, but also has systemic and better residual activities. The production method of epoxiconazole emulsifiable oil is as follows: use fluorobenzene and o-chlorobenzyl chloride as starting materials to synthesize 1-bromo-3-chloro-1-(2-chlorophenyl)-2-(4-fluorophenyl)- ...

Claims

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Application Information

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IPC IPC(8): C07C25/24C07C17/38
CPCC07B2200/09C07C17/38C07C25/24
Inventor 孙伯旺赵雨梦王明亮朱岭军孙晨洪丹丽
Owner SOUTHEAST UNIV
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