170917-89-2Relevant articles and documents
Preparation method of indoxacarb key intermediate
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Paragraph 0007; 0025-0026; 0028-0032; 0034-0038; 0040-0044, (2020/11/05)
The invention belongs to the field of chemical synthesis, and relates to a novel method for preparing an indoxacarb key intermediate. The key intermediate is 7-indeno [1, 2, e] [1, 3, 4] oxadiazine-2,4a (3H, 5H)-dicarboxylic acid-4a-methyl ester-2-benzyl ester. The preparation method is mainly characterized in that a phase transfer catalyst is added in the condensation reaction process, reactantsare in full contact under the action of the phase transfer catalyst, so that the reaction quickly realizes a homogeneous system, the reaction is more thorough, the product yield is high, the reactiontime is shortened by about 3-4 hours compared with the existing process, and the reaction rate is greatly improved. More importantly, the condensation system is a homogeneous system, is easy to dropwise add in the cyclization reaction process, does not block a bottom valve or a pipeline, is convenient to operate, saves manpower and material resources, and is beneficial to industrial production.
Preparation method of indoxacarb intermediate
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Paragraph 0015-0024, (2017/06/02)
The invention relates to a preparation method of indoxacarb intermediate. The preparation method is characterized by comprising the following steps: dissolving intermediate 5-chloro-2-methoxycarbonyl-2-hydroxy-1-indanone into xylene, adding benzyl carbazate and phosphorus pentoxide, separating out phosphoric acid, adding diethoxymethane into reaction liquid, enabling the solvent xylene to flow back on a tower, dropping the obtained reaction liquid into xylene at a constant speed, gathering ethyl alcohol, performing negative pressure desolventizing on obtained reaction liquid, adding a crystallizing agent into the rest liquid, performing cooling crystallization, filtering, and drying, so as to obtain 7-chloroindeno [1,2-e][1,3,4] oxadiazine-2,4a (3H,5H)-dicarboxylicacid-4a-methyl-2-benzylester. The method is convenient to operate, increases the reaction temperature, accelerates the reaction speed, and obviously improves the content and the yield of the intermediate.