Scale synthesis process of procymidone original drug of efficient agricultural bactericide in two steps
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A technology for agricultural fungicide and procymidone technical medicine, which is applied in the field of large-scale synthesis process of high-efficiency agricultural fungicide procymidone, and can solve the problems of high production cost, high sewage discharge, restricting product scale, industrial production and the like. , to achieve the effect of improving performance and use effect, reducing sewage discharge and reducing equipment investment
Inactive Publication Date: 2010-12-08
陕西亿农高科药业有限公司
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In the specific implementation, the above-mentioned three-step synthesis process correspondingly has defects such as complex process route, large equipment investment, low yield, high sewage discharge, high production cost and certain danger in the synthesis process, which restricts it to a large extent. Large-scale and industrialized production of products
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[0013] The content of the present invention will be further described below in conjunction with the embodiments.
[0014] The present invention adopts a two-step large-scale synthesis process to prepare the procymidone original drug, comprising: the first step, using methyl α-chloropropionate and methyl methacrylate to synthesize the intermediate three-membered cyclic ester, and the second step, Procymidone is produced by reacting three-membered cyclic ester with 3,5-dichloroaniline and 70% sulfuric acid.
[0015] One, the process step of utilizing α-methyl chloropropionate and methyl methacrylate to synthesize the intermediate three-membered cyclic ester is:
[0016] 1. Methyl α-chloropropionate, methyl methacrylate and toluene (solvent) are treated with anhydrous NaSO4 to remove water respectively, and set aside;
[0017] 2. Clean the reaction kettle with industrial acetone, then dry the reaction kettle with nitrogen, and set aside;
[0018] 3. Add 0.2 to 0.3 tons of catal...
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Abstract
The invention relates to a scale synthesis process of a procymidone original drug of an efficient agricultural bactericide, which adopts a scale synthesis process in two steps: firstly, synthesizing alpha-propionate methyl chlorine and methacrylate methyl into a midbody of three-membered ring ester under the action of a catalyst of sodium hydride; and secondly, reacting equimolar three-membered ring ester and 3,5-dichloroaniline with 70% of vitriol to generate procymidone. Compared with the prior art, the synthesis process of the invention is simple, reduces the equipment investment of production line and sewage drainage, largely reduces the cost, reduces risk in the synthesis course, establishes the foundation for industrial production, and also obviously enhances performance and use effect of products.
Description
technical field [0001] The content of the invention belongs to the technical field of preparation of agricultural fungicides, and relates to a large-scale synthesis process of high-efficiency agricultural fungicide procymidone. Background technique [0002] Procymidone, also known as procymidone, samidone, dimethyridine, etc., its molecular formula is C 12 h 11 Cl 2 NO 2 , is a low-toxic fungicide with outstanding protective effect on crops and long-lasting effect. After spraying, it can be quickly absorbed by the leaves and roots of crops. It is suitable for fruit trees, vegetables, field crops and ornamental plants, and can effectively control sclerotinia Sclerotinias pp., Botrytis spp. and Cochliobolus spp., such as for the control of gray mold of cucumber, eggplant, tomato, onion, grape, flowers, beans, lettuce, Capsicum stem rot, peach brown rot, large leaf spot, etc. In the prior art both at home and abroad, the preparation of procymidone mainly adopts a three-ste...
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