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Synthesis method of bentazone midbody 2-amino-N-isopropylbenzamide

A technology of isopropyl benzamide and synthesis method, which is applied in the field of synthesis of bentazone intermediate 2-amino-N-isopropyl benzamide, can solve the problem of large investment, large loss of isatoic anhydride, and difficulty in feeding and other issues to achieve the effect of reducing production costs, reducing production processes, and reducing labor

Active Publication Date: 2011-02-09
HEFEI XINGYU CHEM
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Problems solved by technology

[0009] 3) Generally, it is difficult to meet the production requirements for the water content after recovery of dichloroethane, and reducing the water content requires greater investment;
[0010] 4) After drying, the loss of isatoic anhydride is large during production and feeding, and it is difficult for employees to feed (after drying, the material is finer, it is not easy to feed, and it is easy to drift outward

Method used

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  • Synthesis method of bentazone midbody 2-amino-N-isopropylbenzamide

Examples

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Effect test

Embodiment 1

[0015] 1) Put 2800L recovered dichloroethane in the static tank for 1 to 2 hours, and add it into the 5000L reactor equipped with anchor stirring to measure the water content to be 0.3% after water separation;

[0016] 2) Add 900 kilograms of water containing 35% undried isatoic anhydride in the reactor under stirring;

[0017] 3) Heating the reaction system to 50-52° C., and evenly adding 300 kg of isopropylamine dropwise within 3 hours. After dripping, keep the reaction temperature and continue to stir for 1 hour, then add 300 kg of water in two times to wash, divide the water, remove part of dichloroethane, and obtain an amide solution with a content of about 25% and a yield of about 93%. The follow-up production process of grass pine.

Embodiment 2

[0019] 1) Put 2800L of recovered dichloroethane in the static tank for 1 to 2 hours, measure the water content of 0.5% after water separation, and add it to the 5000L reactor equipped with anchor stirring;

[0020] 2) Add 900 kilograms of water in 25% undried isatoic anhydride in the reactor under stirring;

[0021] 3) The reaction system was heated to 56-60° C., and 300 kg of isopropylamine was evenly added dropwise within 3 hours. After dripping, keep the reaction temperature and continue to stir for 1 hour, then add 300 kg of water in two times to wash, divide the water, remove part of dichloroethane, and obtain an amide solution with a content of about 20% and a yield of about 94%. The follow-up production process of grass pine.

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Abstract

The invention discloses a synthesis method of a bentazone midbody 2-amino-N-isopropylbenzamide, comprising the steps of: dripping isopropylamine in a dichloroethane solution of isatoic anhydride within 3 hours at a temperature of 50-60 DEG C, continuing the reaction for 0.5-2 hours at the temperature of 50-60 DEG C, washing with water and distributing water to obtain the 2-amino-N-isopropylbenzamide, wherein the water content of the isatoic anhydride is not higher than 40% and the water content of the dichloroethane is not higher than 1%. The synthesis method of the bentazone midbody 2-amino-N-isopropylbenzamide in the invention is free from anhydrous rigorous reaction conditions to be controlled strictly, greatly decreases the production processes, lightens the labor capacity of operators, saves the energy, reduces the consumption and the production cost.

Description

technical field [0001] The invention relates to the technical improvement of the amide reaction in the production process of the bentazone technical substance, in particular to the synthesis method of the bentazone intermediate 2-amino-N-isopropylbenzamide. Background technique [0002] Bentazone has another name called bentazone, which is a broad-spectrum, contact systemic conduction herbicide, wherein the synthetic reaction formula of the raw material intermediate 2-amino-N-isopropylbenzamide is: [0003] [0004] Isatoic anhydride Isopropylamine [0005] Traditionally, this reaction requires the dichloroethane system to be absolutely anhydrous. For example, fresh anhydrous dichloroethane must be used, and isatoic anhydride must also be dried in a dryer. The reaction process is as follows: first add fresh anhydrous dichloroethane into the reactor equipped with paddle stirring, then add the dried isatoic anhydride, add isopropylamine dropwise at 30-40°C, and add dropwis...

Claims

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Application Information

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IPC IPC(8): C07C237/30C07C231/14
Inventor 丁云好姚海波王传品王兰兰赵国霞
Owner HEFEI XINGYU CHEM
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