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Method for separating chiral compound metalaxyl by adopting simulated moving bed in fourth region

A technology for simulating moving bed and metalaxyl, applied in the field of simulated moving bed chromatographic separation of metalaxyl, can solve problems such as being in the analysis stage, and achieve the effects of stable product quality, continuous automation of production, and simple process

Inactive Publication Date: 2013-03-06
江苏汉邦科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although metalaxyl has entered the Chinese market since the mid-1980s, the research on its split is still in the analysis stage

Method used

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  • Method for separating chiral compound metalaxyl by adopting simulated moving bed in fourth region
  • Method for separating chiral compound metalaxyl by adopting simulated moving bed in fourth region

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach

[0029] 1. Preparation of cellulose-tris(3,5-dimethylphenylcarbamate) filler

[0030] Prepare according to the method of literature (Okamoto Y, Kawashima M, Hatada K J . Chromatogr.1986,363:173~186). Cellulose and phenyl isohydrogen were reacted in pyrrole solution at 100° C. for 24 hours, and the methanol-insoluble product obtained from the reaction was cellulose-tris(3,5-dimethylphenylcarbamate). Cellulose-tris(3,5-dimethylphenylcarbamate) was dissolved in tetrahydrofuran, and aminopropyl silica gel was added to the solution, and electromagnetically stirred until the tetrahydrofuran was volatilized, and repeated 3 times to obtain cellulose- Tris(3,5-dimethylphenylcarbamate) coated chiral stationary phase. Wherein the weight ratio of cellulose-three (3,5-dimethylphenylcarbamate) to aminopropyl silica gel is 1:5;

[0031] 2. Selection of mobile phase

[0032] The composition of the mobile phase affects the separation of metalaxyl enantiomers, and also affects the productivit...

example 1

[0053] A operating conditions

[0054] Mobile phase: methanol: water = 15:85

[0055] Injection concentration: 7mg / ml

[0056] Injection liquid flow rate: 2.5 ml / min

[0057] Eluent flow rate: 1.0 ml / min

[0058] Extraction flow rate: 1.5 ml / min

[0059] Raffinate flow rate: 2.0 ml / min

[0060] Switching time: 6.8min

[0061] System temperature: 25°C

[0062] B finished product analysis

[0063] Analyzing the composition of the extract and raffinate with an analytical column, the purity of the extract is 99.3%, and the purity of the raffinate is 99.1%. Each kilogram of stationary phase can produce 0.3kg of R-metalaxyl and S-metalaxyl each day , the mobile phase consumption was 57L / kg, and the recovery rate was 95.2%;

example 2

[0065] A operating conditions

[0066] Mobile phase: methanol: water = 20:80

[0067] Injection concentration: 10mg / ml

[0068] Injection liquid flow rate: 6.0 ml / min

[0069]Eluent flow rate: 5.0 ml / min

[0070] Extraction flow rate: 4.0 ml / min

[0071] Raffinate flow rate: 6.0 ml / min

[0072] Switching time: 7.5min

[0073] System temperature: 20°C

[0074] B finished product analysis

[0075] Analyzing the composition of the extract and raffinate with an analytical column, the purity of the extract is 99.5%, and the purity of the raffinate is 99.3%. Each kilogram of stationary phase can produce 0.53kg of R-metalaxyl and S-metalaxyl each day , the mobile phase consumption was 83.3L / kg, and the recovery rate was 98.1%.

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Abstract

The invention discloses a method for separating chiral compound metalaxyl by adopting a simulated moving bed in a fourth region. The method is characterized by adopting a simulated moving bed chromatography system, taking cellulose-tris(3,5-dimethylphenylcarbamate) as a filler and methanol and water as mobile phases and separating high-purity R-metalaxyl and S-metalaxyl from racemes of metalaxyl. The simulated moving bed chromatography system has the advantages of continuous production, high degree of automation and high production efficiency.

Description

technical field [0001] The invention relates to a separation technology of chiral drugs, in particular to a simulated moving bed chromatographic separation method of metalaxyl. Background technique [0002] Metalaxyl (Metalaxy1), the chemical name is N-(2-methoxymethylacetyl)-N-(2,6-dimethylphenyl)-racemic amino acid methyl ester, and its chemical structure is: [0003] [0004] Metalaxyl is a new type of high-efficiency systemic fungicide, which can be absorbed into plants. Its water solubility is much higher than that of general fungicides. It can penetrate into the cell membrane of oomycetes with small lipids and play a bactericidal effect. The downy mildew and Phytophthora have selective effects, such as potato late blight, grape downy mildew, hop downy mildew, sugar beet blight, rapeseed white rust, tobacco black shank, etc. have good control effects. It can be used for downy mildew of melons, vegetables, grapes, tobacco, etc., potato late blight, tobacco black dis...

Claims

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Application Information

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IPC IPC(8): C07C235/16C07C231/20B01D15/10
Inventor 李胜迎李枝玲金新亮初新王冰冰居延娟
Owner 江苏汉邦科技股份有限公司
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