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Fluroxypyr sec-octyl ester synthesizing method

A technology of fluroxypyr sec-octyl ester and synthesis method, applied in the direction of organic chemistry, etc., to achieve the effect of high yield

Inactive Publication Date: 2014-05-14
JIANGSU INST OF ECOMONES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Fluroxypyr sec-octyl ester products have domestic research reports on its use and application methods, but no reports on its synthesis methods have been seen.

Method used

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Examples

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Embodiment

[0013] Potassium 4-amino-3,5-dichloro-6-fluoro-2-pyridinate was dissolved in N-methylpyrrolidone (NMP), and the water was distilled under reduced pressure to below 500ppm. Add excess methyl chloroacetate and stir to raise the temperature, maintain the temperature until 4-amino-3,5-dichloro-6-fluoro-2-pyridinol potassium is completely reacted, the reaction time is 5-5.5 hours, and the reaction temperature is 52-55°C After the reaction is completed, distill off the remaining methyl chloroacetate, pour an appropriate amount of water into the reaction solution, stir and heat to 80-85°C for 1-2 hours, then put it in ice water to cool and crystallize, wait until the product is completely precipitated, filter and wash, dry After drying, a white solid was obtained with a yield of 95.6% and a content of 99.2%.

[0014] The molar ratio of N-methylpyrrolidone (NMP) to potassium 4-amino-3,5-dichloro-6-fluoro-2-pyridinol is 8-9: 1,4-amino-3,5-dichloro-6- The reaction molar ratio of potass...

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Abstract

A fluroxypyr sec-octyl ester synthesizing method comprises the following steps that (1) 4-amino-3,5-dichloro-6-fluorine-2-pyridine potassium phenoxide is dissolved in N-methyl pyrrolidone, an excessive amount of methyl chloroacetate is added into the solution, and stirring and temperature rising are conducted for reaction, wherein the reaction time is 5-5.5 hours and the reaction temperature is 52 DEG C-55 DEG C; (2) an excessive amount of sec-octyl ester and 4-amino-3,5-dichloro-6-fluorine-2 pyridine oxygen methyl acetate are mixed and stirred and o.5%-1% of butyl titanate is added, wherein the alcohol and ester molar ratio is 2-2.3:1, the reaction temperature is 115 DEG C and the reaction time is 4-4.5 hours; after reaction ends, fluroxypyr sec-octyl ester is obtained.

Description

technical field [0001] The invention relates to a method for synthesizing fluroxypyr sec-octyl ester. Background technique [0002] The chemical name of fluroxypyr sec-octyl ester is 4-amino-3,5-dichloro-6-fluoro-2-pyridyloxyacetic acid (1-methylheptyl ester), with a melting point of 56-57°C and a stable storage period at room temperature For two years, it decomposes above the melting point, and the industrial raw material is a white crystal with a soapy smell. Fluroxypyr sec-octyl ester is a herbicide with systemic conductivity, which can be used as post-emergence stem and leaf treatment, suitable for a variety of crops, such as wheat, barley, corn, orchard and other winter crops, to control a variety of malignant weeds Ashamed, such as pig vines, water peanuts, field bindweed and so on. Fluroxypyr sec-octyl ester product has domestic research reports on its use and application method, but no report on its synthesis method has been seen. Contents of the invention [00...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/73
CPCC07D213/73
Inventor 孔繁蕾张旺庚丁武松
Owner JIANGSU INST OF ECOMONES
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