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Novel synthetic technology of nicosulfuron

A technology of nicosulfuron and a new process, applied in the direction of organic chemistry, etc., can solve the problems of reducing the separation effect of the rectification tower, low yield and content, and long reaction time, so as to shorten the reaction time, reduce production costs, The effect of product yield and content improvement

Inactive Publication Date: 2013-12-18
ANHUI FENGLE AGROCHEM
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Problems solved by technology

Since part of the ethanol circulates at the top of the tower, and the rectification tower uses an external reflux method, the reflux liquid is relatively supercooled, which reduces the separation effect of the rectification tower. Therefore, the process has a long reaction time, high energy consumption, and the yield and The content is not high

Method used

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  • Novel synthetic technology of nicosulfuron

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Experimental program
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Effect test

Embodiment

[0007] Embodiment: a kind of nicosulfuron synthetic new technique, operation is as follows:

[0008] In the 2000L reactor with internal reflux (①) rectifying tower, drop into the urethane of 0.5kmol, the pyrimidinamine of 0.6kmol and 1000L toluene, be warmed up to reflux, control tower top temperature, pass atomizing nozzle ( ②) Pass in atomized water droplets, and at the same time separate the water phase containing ethanol in the lower layer of the oil-water separator (③), and return the upper organic phase to the top of the rectification tower. After reacting for about 4 hours, take the water phase to detect the ethanol content, and stop after passing the test. Reaction, crystallization at lower temperature, filtration, washing, and drying to obtain the product with a content of 98.1% and a yield of 98.2%.

[0009]

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Abstract

The invention provides a novel synthetic technology of nicosulfuron. A rectifying tower for separating a by-product ethanol in the technology employs an internal reflux way; and a mode of introducing atomized water droplets into a gas pipeline on the upper portion of the rectifying tower is used for extracting ethanol. The product content reaches higher than 98%, and a yield reaches higher than 98%.

Description

technical field [0001] The invention belongs to the technical field of pesticides, and in particular relates to a new process for synthesizing nicosulfuron. Background technique [0002] At present, the large-scale production and synthesis process of nicosulfuron basically uses 2-ethoxycarbonylaminosulfonyl-N,N-dimethylnicotinamide (referred to as urethane) and pyrimidinamine to condense in a solvent to remove a molecule of ethanol The method is to separate ethanol by rectification, adopting the method of extracting part of the solvent containing ethanol from the top of the tower and adding fresh solvent to the reaction kettle in equal amounts. Since part of the ethanol circulates at the top of the tower, and the rectification tower uses an external reflux method, the reflux liquid is relatively supercooled, which reduces the separation effect of the rectification tower. Therefore, the process has a long reaction time, high energy consumption, and the yield and The content ...

Claims

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Application Information

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IPC IPC(8): C07D401/12
Inventor 周康伦苏朝辉金劲松章昆仑林昌志施亦敏凌朵朵陈克付
Owner ANHUI FENGLE AGROCHEM