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A technology for the preparation of methoxyfenozide, which is applied in the field of preparation of methoxyfenozide, can solve the problems of increasing the production burden of enterprises, high production costs, and difficult sewage discharge, and achieves the reduction of wastewater treatment difficulty and the reaction process. Convenience and the effect of reducing production costs
Inactive Publication Date: 2017-05-24
JIANGSU YONGAN CHEM CO LTD
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However, most of the existing methoxyfenozide is prepared in an assembly line, the production cost is relatively high, and a large amount of waste wat
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[0006] The technical solution adopted in the present invention is: the preparation process of methoxyfenozide, including the following steps: (1) Condensation reaction: at room temperature, add tert-butylhydrazine hydrochloride and dichloroethane into the condensation kettle, clamp Cool the frozen brine to -6~-5°C, add liquid caustic soda dropwise, let it stand for stratification, separate the water layer to waste water treatment, keep the organic layer at this temperature, add 3-methoxy-2-methylbenzene dropwise Formyl chloride, control the dropping rate, so that the temperature of the kettle does not exceed 0°C; after 7-9 hours of reaction, the sampling analysis is qualified, then add water to stir, static layering, the water layer is sent to waste water treatment, and the organic layer is kept at a normal temperature of 75-85°C. Dichloroethane is released under high pressure, and toluene is added after cooling down to room temperature to dissolve, and the toluene liquid of th...
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Abstract
The invention discloses a preparation process of methoxyfenozide. The process comprises steps as follows: (1) a condensation reaction: tert-butylhydrazine hydrochloride and dichloroethane are added to a condensation kettle at the room temperature, a jacket is cooled to subzero 6 DEG C to subzero 5 DEG C with brine freezing water, a caustic soda liquid is dropwise added, the mixture is left to stand for layering, a water layer is separated out for wastewater treatment, an organic layer is kept at the temperature, 3-methoxy-2-methoxybenzoyl chloride is dropwise added, and the dropwise adding speed is controlled, so that the temperature of the kettle does not exceed 0 DEG C; after a reaction is performed for 7-9 h, if sampling analysis proves qualification, water is added for stirring again, the mixture is left to stand for layering, the water layer is sent for wastewater treatment, dichloroethane is separated out from the organic layer at 75-85 DEG C under the normal pressure condition, toluene is added for dissolution after the mixture is cooled to the room temperature, and a toluene solution of a condensation compound is obtained.
Description
technical field [0001] The invention relates to a preparation process of methoxyfenozide. Background technique [0002] Methoxyfenozide is a new type of specific phenylhydrazide insecticide with low toxicity, mainly used to control the larvae of Lepidoptera pests, such as beet armyworm, cabbage armyworm, litura, cabbage insect, cotton boll Insects, golden leaf moths, American white moths, pine caterpillars, inchworms and rice borers, etc., suitable for crops such as cruciferous vegetables, solanaceous vegetables, melons, cotton, apples, peaches, rice, forest trees, etc., its high efficiency The performance and environmental friendliness meet the requirements and development trends of modern pesticides. However, most of the existing methoxyfenozide is prepared in an assembly line, the production cost is relatively high, and a large amount of wastewater is generated during the production process, making it difficult to discharge the sewage, which further increases the product...
Claims
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