170917-89-2Relevant academic research and scientific papers
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 key intermediate
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Paragraph 0048; 0051-0054; 0057-0059, (2020/07/02)
The invention belongs to the field of chemical synthesis, and relates to a novel preparation method of an indoxacarb key intermediate. In the cyclization reaction process of the key intermediate synthesis method, paraformaldehyde substances are adopted to replace original diethoxymethane, generation of by-product ethanol in the reaction process is avoided, generation of ethyl ester impurities is effectively inhibited, generation of a mixed solvent is eliminated, the environmental protection pressure is reduced, the production cost is greatly reduced while the quality of the intermediate is improved, and a good foundation is laid for production of high-quality indoxacarb.
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.
Bromodimethyl sulfonium bromide mediated rapid and facile protection of amines
Shailaja,Manjula,Vittal Rao
experimental part, p. 2073 - 2080 (2011/07/31)
A new clean protocol for protection of aryl and aliphatic amines with t-butoxycarbonyl (t-BOC) and benzyloxycarbonyl (Cbz) catalyzed by simple (bromodimethyl) sulfonium bromide has been developed. Rapid protection of amines in excellent yields in totally solvent-free conditions has been achieved. Copyright
