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Synthesizing method for pesticide intermediate 4-formyl menthyl valerate

A technology for the synthesis of methyl formyl valerate and a synthesis method, which is applied in the field of synthesis of methyl 4-formyl valerate, a pesticide intermediate, can solve the problems of difficult recovery of raw material morpholine and difficulty in meeting environmental protection requirements, and achieve convenient and continuous The effects of efficient production, easy separation, and convenient recycling

Active Publication Date: 2018-06-08
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The morpholine salt solution needs to be strengthened with alkali sodium hydroxide or potassium hydroxide to adjust the pH ≥ 10 to recover morpholine freely. It is difficult to recover raw material morpholine in industrial production, and a large amount of high-salt wastewater is produced, which is difficult to meet the requirements of environmental protection.

Method used

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  • Synthesizing method for pesticide intermediate 4-formyl menthyl valerate
  • Synthesizing method for pesticide intermediate 4-formyl menthyl valerate
  • Synthesizing method for pesticide intermediate 4-formyl menthyl valerate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preheating

[0031] Add pretreated strong acidic resin D072 and deionized water to a fixed-bed reactor with an inner diameter of 4cm and a height of 40cm. The resin filling height is 32cm (about 300g in weight), and the mixture in the reactor is heated to 50°C; (2) Acid hydrolysis

[0032] After the temperature of the material in the reactor in step (1) is stable, the 755.7g cyclobutane (content 84.56%) and deionized water in the raw material storage tank are continuously injected into the reactor with a metering pump to adjust the space velocity of the cyclobutyl 0.2h -1 , deionized water space velocity 0.2h -1 , control the temperature of the fixed bed at 50°C, the reaction process can be sampled and analyzed, and the cyclobutane content is normalized by gas chromatography to analyze 0.2%; when the reaction liquid sampling gas chromatography analyzes the cyclobutane normalized content > 2%, the resin needs to be regenerated After treatment, it will continue to ...

Embodiment 2

[0037] (1) Preheating

[0038] Add pretreated strong acid resin D072 and deionized water to a fixed-bed reactor with an inner diameter of 4 cm and a height of 40 cm. The resin filling height is 32 cm (weight is about 300 g), and the mixture in the reactor is heated to 75 ° C;

[0039] (2) Acid hydrolysis

[0040] After the temperature of the material in the reactor of step (1) is stable, the 1997.6g cyclobutane (content 85.3%) and deionized water in the raw material storage tank are continuously injected into the reactor with a metering pump, and the space velocity of the cyclobutyl substance is adjusted 1h -1 , deionized water space velocity 0.8h -1 , control the temperature of the fixed bed at 75°C, the reaction process can be sampled and analyzed, and the cyclobutane content is normalized to 0.4% by gas chromatography; when the reaction liquid sampling gas chromatography analyzes the cyclobutane normalized content > 2%, the resin needs to be regenerated After treatment, ...

Embodiment 3

[0045] (1) Preheating

[0046] Add pretreated strong acid resin D072 and deionized water to a fixed-bed reactor with an inner diameter of 4 cm and a height of 40 cm. The resin filling height is 32 cm (weight is about 300 g), and the mixture in the reactor is heated to 65 ° C;

[0047] (2) Acid hydrolysis

[0048] After the temperature of the material in the reactor in step (1) is stable, the 1259.5g cyclobutane (content 84.56%) and deionized water in the raw material storage tank are continuously injected into the reactor with a metering pump to adjust the space velocity of the cyclobutane 0.5h -1 , deionized water space velocity 0.2h -1 , control the fixed bed temperature at 65°C, sample analysis can be done during the reaction, and use gas chromatography to analyze the normalized content of cyclobutane at 0.45%. After treatment, it will continue to be used for acid hydrolysis after regeneration.

[0049] The reaction solution enters the tower from the feed port (20cm awa...

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Abstract

The invention belongs to the technical field of organic chemicals, and relates to a synthesizing method for a pesticide intermediate 4-formyl menthyl valerate, more particularly to a method for synthesizing amyl ester by taking 3-methyl-2-(4-morpholinyl)methyl cyclobutyrate as a raw material and performing catalytic acidolysis by using highly acidic resin. The yield of the amyl ester is not less than 80 percent; a byproduct morpholine exists in a reaction liquid in a free state; the morpholine is recycled through a commonly used chemical operating unit. The synthesizing method for the pesticide intermediate 4-formyl menthyl valerate has the advantages of that an operation process is simple and continuous, morpholine serving as the raw material is convenient to recover, equipment is not corroded, the industrial wastewater amount is small, and the product yield is high.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, relates to a kind of synthetic method of pesticide intermediate 4-formyl valerate methyl ester (abbreviation: pentyl ester); -Morpholinyl) methyl cyclobutyrate (abbreviation: cyclobutane) as raw material, use strong acidic resin to catalyze acidolysis to synthesize pentyl ester, the yield of pentyl ester is not less than 80%, and the by-product morpholine exists in free state In the reaction solution, morpholine is recovered through common chemical unit operations. The present invention has the advantages of simple and continuous process operation, convenient recovery of raw material morpholine, no corrosion of equipment, less industrial waste water, high product yield and the like. Background technique [0002] Methyl 4-formylvalerate, the structure of which is shown in formula (1), is a precursor of 2-chloro-5-picoline, an important intermediate for the synthesis of pyridine ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/313C07C67/54
CPCC07C67/313C07C67/54C07C69/716
Inventor 周颖华史雪芳丁克鸿徐林田宇汪洋聂庆超徐浩
Owner JIANGSU YANGNONG CHEM GROUP
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