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Method for preparing oxaziclomefone

A technology of oxaziclozone and its compound, which is applied in the field of preparing oxaziclomem, can solve the problems of complex process route, low product purity, and unsuitability for large-scale industrial production, and achieve the effect of simple process steps and low cost

Active Publication Date: 2020-06-26
SHANDONG CYNDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The object of the present invention is to provide a new method for preparing oxazicone suitable for industrial production in view of the defects of complicated process route, low purity of the obtained product and unsuitability for large-scale industrial production in the method for preparing oxazicone in the prior art. Keto method to obtain high purity oxaziclozone

Method used

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  • Method for preparing oxaziclomefone
  • Method for preparing oxaziclomefone
  • Method for preparing oxaziclomefone

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Oxaziclozone having the structure represented by formula (1) was prepared.

[0047] 1) At 0°C, add the compound (0.1mol), phenylacetonitrile (0.11mol) and toluene (100mL) represented by formula (1-1) into the reaction flask, stir well, add concentrated sulfuric acid (98 wt. %, the same below) total 20g, and control the speed of dripping the concentrated sulfuric acid so that the liquid temperature in the reaction bottle is not higher than 10°C, after the dropwise addition of the concentrated sulfuric acid, continue to react for 8h (start timing from the beginning of the dripping of the concentrated sulfuric acid), and then Add 100 mL of water to the reaction system, add aqueous sodium carbonate solution dropwise until the pH of the solution is 7, filter, and dry to obtain the compound shown in formula (1-2), with a yield of 94.4% and a purity of 93.9%;

[0048]2) At 0°C, sodium methoxide (0.2mol) and methyl acetate (2.5mol) were added to the reaction flask, stirred even...

Embodiment 2

[0051] Oxaziclozone having the structure represented by formula (1) was prepared.

[0052] 1) At -4°C, add the compound (0.1mol), phenylacetonitrile (0.12mol) and toluene (100mL) represented by formula (1-1) into the reaction flask, stir well, add concentrated sulfuric acid (98 % by weight, the same below) is 18g in total, and the speed of dripping the vitriol oil is controlled so that the liquid temperature in the reaction bottle is not higher than 10°C, and after the vitriol dripping, continue to react for 12h (starting to count from the vitriol dripping), Then add 100mL water to the reaction system, add dropwise sodium carbonate aqueous solution until the pH value of the solution is 7, filter and dry to obtain the compound shown in formula (1-2), with a yield of 96.5% and a purity of 96.2%;

[0053] 2) At -10°C, add sodium ethoxide (0.3mol) and ethyl acetate (2.5mol) into the reaction flask, stir evenly, and add dropwise the ethyl acetate solution containing the compound re...

Embodiment 3

[0056] The present embodiment adopts the method similar to embodiment 1 to carry out, and the difference is, in the step 2) of the present embodiment, control the speed of dripping the methyl acetate solution containing the compound shown in formula (1-2) so that the reaction The liquid temperature in the bottle is not higher than 20°C.

[0057] As a result, the yield of the compound shown in formula (1-3) was 85.1%, and the purity was 97.2%;

[0058] The same method as in Example 1 was used to prepare oxaziclozone represented by formula (1) from the compound represented by formula (1-3) in this example, with a yield of 74% and a purity of 95.7%.

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Abstract

The invention relates to the field of organic synthesis, and discloses a method for preparing oxaziclomefone, which comprises: 1) carrying out first contact on a compound represented by a formula (1-1) and phenylacetonitrile under an acidic condition to obtain a compound represented by a formula (1-2); 2) under an alkaline condition, carrying out second contact on the compound shown in the formula(1-2) and methyl acetate to obtain a compound shown in a formula (1-3); and 3) in the presence of a catalyst, carrying out third contact on the compound represented by the formula (1-3) and a methyldonor. According to the method provided by the invention, high-purity oxaziclomefone can be obtained on the premise of not using a purification means of column chromatography, so that the method provided by the invention is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for preparing oxaziclozone. Background technique [0002] Weeds in rice fields are undesirable because they harm the growth of rice and affect the yield of rice. Many herbicides suitable for controlling weeds in paddy fields have been developed, and many herbicides have also been widely used in the control of weeds in paddy fields. However, there are many kinds of weeds in paddy fields with different characteristics, and the harm to rice growth and the stages of harm are also different. [0003] Oxazimidone is a beneficial broad-spectrum herbicide. [0004] However, the method for preparing oxaziclomele disclosed in the prior art has the disadvantages of complex process route and low purity, requiring purification by column chromatography, which will cause a large loss of the product and increase the production cost. [0005] This has limited the wide commercial appli...

Claims

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Application Information

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IPC IPC(8): C07D265/06
CPCC07D265/06
Inventor 王现全李凯邹亚波宋萍
Owner SHANDONG CYNDA CHEM
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