Synthesis method of fenpropimorph

A synthesis method and technology of fenpropimorph are applied in the field of synthesis of fenpropimorph, can solve problems such as no industrial production value, and achieve the effects of low cost, simple equipment and high content of finished products

Active Publication Date: 2015-05-20
NANTONG WEILIKE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

No industrial production value

Method used

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  • Synthesis method of fenpropimorph
  • Synthesis method of fenpropimorph
  • Synthesis method of fenpropimorph

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Add 206g of p-tert-butyl-β-methylphenylpropanol and 120g of methanesulfonyl chloride into a 500ml round-bottomed flask, cool down to 0°C, add 111g of triethylamine dropwise, and keep the temperature for 1 hour after the dropwise addition is complete. Sampling and analysis until qualified. Add 200g of water after the heat preservation finishes, let stand and separate. The lower layer is the intermediate sulfonate after reaction. Weighed 282.6g of the intermediate, and the analytical content (GC normalization method) was 99.0%. The yield is 99.5%.

[0029] Put the sulfonate ester synthesis product of the first step into a 1000ml four-necked flask, add 345g of 2,6-dimethylmorpholine, heat up and reflux until the temperature rises to 140°C, keep it warm for 4 hours, and then neutralize it with 30% NaOH aqueous solution To PH = 14, static separation, the upper oil layer vacuum distillation, after cutting off the former fraction to collect the finished fenpropimorph. Weig...

Embodiment 2

[0031] Add 103g of p-tert-butyl-β-methylphenylpropanol and 60g of methanesulfonyl chloride into a 500ml round bottom flask, cool down to 0°C, add 56g of triethylamine dropwise, and keep the temperature for 1 hour after the dropwise addition is complete. Sampling and analysis until qualified. Add 100g of water after the heat preservation finishes, and let stand to stratify. The lower layer is the intermediate sulfonate after reaction. 141.4 g of the intermediate was obtained by weighing, and the analytical content (GC normalization method) was 98.9%. The yield is 99.5%.

[0032] Put the sulfonate ester synthesis product of the first step into a 500ml four-neck flask, add 173g of 2,6-dimethylmorpholine, heat up and reflux until the temperature rises to 140°C, keep it warm for 4 hours, and then neutralize it with 30% NaOH aqueous solution To PH = 14, static separation, the upper oil layer vacuum distillation, after cutting off the former fraction to collect the finished fenpro...

Embodiment 3

[0034] Add 412g of p-tert-butyl-β-methylphenylpropanol and 240g of methanesulfonyl chloride into a 1000ml round bottom flask, cool down to 0°C, add 222g of triethylamine dropwise, and keep the temperature for 1 hour after the dropwise addition. Sampling and analysis until qualified. Add 400g of water after the heat preservation finishes, and let stand to stratify. The lower layer is the intermediate sulfonate after reaction. 567.4g of the intermediate was obtained by weighing, and the analytical content (GC normalization method) was 98.5%. The yield is 99.4%.

[0035] Put the sulfonate ester synthesis product of the first step into a 2000ml four-necked flask, add 690g of 2,6-dimethylmorpholine, raise the temperature and reflux until the temperature rises to 140°C, keep it warm for 4 hours, and then neutralize it with 30% NaOH aqueous solution To PH = 14, static separation, the upper oil layer vacuum distillation, after cutting off the former fraction to collect the finished...

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Abstract

The invention discloses a synthesis method of fenpropimorph. The method adopts p-tert-butyl-beta-methylphenylpropanol as a start raw material and comprises the following steps of: performing esterification by use of methylsufonyl chloride or performing chlorination by use of thionyl chloride to synthesize an intermediate; and synthesizing by use of the intermediate and 2,6-dimethylmorpholine to generate fenpropimorph. The method disclosed by the invention has the advantages of high reaction yield, no environmental pollution, high finished product content, simple process, industrial production value, easiness in operation, simple equipment, few three wastes, low cost and the like.

Description

technical field [0001] The invention relates to a method for synthesizing fenpropimorph. Background technique [0002] Fenpropimorph (Fenpropimorph), also known as Fenpropimorph, Prophyllin, the chemical name is (±) cis 4-[3-(4-tert-butylphenyl)-2-methylpropyl]-2,6 -Dimethylmorpholine, the pure product is a colorless, oily liquid with an aromatic odor, with a boiling point of 392°C (101.3kPa), and is a systemic morpholine fungicide with preventive and therapeutic effects and ergosterol reduction Inhibitors. [0003] The chemical structural formula is: [0004] [0005] The existing domestic synthesis process of fenpropimorph is shown in the figure below: 2-methyl-4-p-tert-butyl benzaldehyde is obtained by condensation with propionaldehyde under alkaline conditions using p-tert-butylbenzaldehyde as the starting material Phenylacrolein, and then undergo selective hydrogenation reduction to obtain 2-methyl-4-p-tert-butylphenylpropanal, and finally react with 2,6-dimethylm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D265/30
Inventor 蒋慧华秦孟云章奉良韩延叁
Owner NANTONG WEILIKE CHEM
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