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Synthesis method of 2-methyl methyl acetoacetate for pesticide production

A technology of methyl methyl acetoacetate and methyl acetoacetate, which is applied in the field of synthesis of methyl 2-methyl acetoacetate for pesticide production, can solve the problems of affecting product market share, poor product quality, and strong odor. Achieve the effects of saving production cost, moderate reaction rate and improving recovery rate

Inactive Publication Date: 2017-01-11
陆开珍
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the process route adopted in the production of hydroxypyrimidine in China is heavily polluted, has a strong odor, and the product quality is also poor, which affects the market share of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of synthetic method of methyl 2-methyl acetoacetate for pesticide production, comprises the steps:

[0024] (1) Raw materials

[0025] Selecting mass fraction is 99% methyl acetoacetate, 2% palladium carbon, acetic acid and pyridine as raw material, the proportioning of described methyl acetoacetate, palladium carbon, acetic acid and pyridine is 1:0.004:0.5:0.5;

[0026] (2) replacement

[0027] The raw materials are added to the autoclave, and then hydrogen gas is introduced into the autoclave, and the material is replaced in the autoclave. The number of times of the replacement is 2 times, and the pressure of the hydrogen is 0.4MPa;

[0028] (3) stirring

[0029] Then formaldehyde was added at 0.1m 3 The speed is evenly injected into the autoclave, then insulated and stirred for 0.5h to obtain the reaction product, the ratio of the formaldehyde and methyl acetoacetate is 1:1.00, and the addition time of the formaldehyde is 3h after the replacement;

[0030]...

Embodiment 2

[0035] A kind of synthetic method of methyl 2-methyl acetoacetate for pesticide production, comprises the steps:

[0036] (1) Raw materials

[0037] Selecting mass fraction as 99% methyl acetoacetate, 3% palladium carbon, acetic acid and pyridine as raw material, the proportioning of methyl acetoacetate, palladium carbon, acetic acid and pyridine is 1:0.005:1.0:1.0;

[0038] (2) replacement

[0039] The raw materials are added into the autoclave, and then hydrogen gas is introduced into the autoclave, and the material is replaced in the autoclave, the number of times of the replacement is 3 times, and the pressure of the hydrogen is 0.5MPa;

[0040] (3) stirring

[0041] Then formaldehyde was added at 0.2m 3 The speed is uniformly injected into the autoclave, then insulated and stirred for 1.0h to obtain the reaction product, the ratio of the formaldehyde and methyl acetoacetate is 1:1.03, and the addition time of the formaldehyde is 4h after the replacement;

[0042] (4) ...

Embodiment 3

[0047] A kind of synthetic method of methyl 2-methyl acetoacetate for pesticide production, comprises the steps:

[0048] (1) Raw materials

[0049] Selecting mass fraction is 99% methyl acetoacetate, 4% palladium carbon, acetic acid and pyridine as raw material, the proportioning of described methyl acetoacetate, palladium carbon, acetic acid and pyridine is 1:0.006:1.5:1.5;

[0050] (2) replacement

[0051] The raw materials are added to the autoclave, and then hydrogen gas is introduced into the autoclave, and the material is replaced in the autoclave. The number of times of the replacement is 4 times, and the pressure of the hydrogen is 0.6MPa;

[0052] (3) stirring

[0053] Then formaldehyde was added at 0.3m 3 The speed is evenly injected into the autoclave, then insulated and stirred for 1.5h to obtain the reaction product, the ratio of the formaldehyde and methyl acetoacetate is 1:1.05, and the addition time of the formaldehyde is 5h after the replacement;

[0054]...

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PUM

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Abstract

The invention discloses a synthesis method of 2-methyl methyl acetoacetate for pesticide production. By means of matching of methyl acetoacetate, palladium on carbon, acetic acid and pyridine, the recovery rate of methyl acetoacetate can be increased while the reaction rate is proper; through control over the ratio of formaldehyde to methyl acetoacetate, the recovery rate of methyl acetoacetate can be increased while quality is guaranteed; through control over the adding time of formaldehyde, the yield of products can be increased, filtered palladium on carbon is recycled, the production cost can be reduced, the vacuum degree ranges from 1,330 Pa to 2,660 Pa, and the effect of reduced pressure distillation can be improved. 2-methyl methyl acetoacetate synthesized through the synthesis method has the advantages of being high in yield and low in cost, market potential is large, and prospects are wide.

Description

technical field [0001] The invention belongs to the field of agricultural production methods, more specifically, the invention relates to a synthetic method of methyl 2-methyl acetoacetate for pesticide production. Background technique [0002] In the past 30 years, pesticide varieties with high efficiency, low toxicity and novel structure have emerged continuously, and their market share has continued to expand. , Pyrimol, Pyrimol Sulfonate, Pyrimol and other global market shares have not declined. The markets of the above-mentioned pesticide varieties are mainly in foreign countries, and the content of harmful impurities needs to be strictly controlled. The key lies in the production of the intermediate hydroxypyrimidine, which directly affects the quality of the pesticide raw material, and its production cost also directly affects the quality of the pesticide raw material. Drug production costs and profits. At present, the production process of hydroxypyrimidine in Chin...

Claims

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Application Information

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IPC IPC(8): C07C67/343C07C67/48C07C69/716
CPCC07C67/343C07C67/48
Inventor 陆开珍
Owner 陆开珍
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