专利号:US-2023303546-A1 优先权日:2020-03-05 标题:Process And Intermediates For The Preparation Of Pyroxasulfone 发明人:RECSEI CARL; BARDA YANIV 权利人:ADAMA AGAN LTD 摘要:The invention relates to a process for preparing a key intermediate of Formula (I) in the synthesis of pyroxasulfone. The process comprises reacting an isoxazole of Formula (II) with a thionating reagent to create an S-substituted thioisoxazole of Formula (III); and combining the S-substituted thioisoxazole of Formula (III) with a pyrazole of the Formula (IV) by introducing a methylene bridge, to obtain a compound of Formula (I). The invention also relates to novel S-substituted thioisoxazole of Formula (III) and processes of preparation thereof, wherein L1 is halogen or an anionic residue derived from an acid; R is an organic residue derived from a suitable thionating reagent: dimethyl thioformamide, thiosulfate salts, dithiooxamide, alkyl xanthate salts, thiobenzamide, V-substituted thiourea and thioacetate salts.
专利号:WO-0107416-A1 优先权日:1999-07-28 标题 :Method of producing pyridazine carboxylic acid derivatives 发明人:BESSARD YVES; CRETTAZ ROGER; EGGEL MICHAEL 权利人:LONZA AG; BESSARD YVES; CRETTAZ ROGER; EGGEL MICHAEL 摘要:The invention relates to a method of producing pyridazine carboxylic acid derivatives of the general formulae (Ia) or (Ib), wherein R<1> represents a group of the formula -OR<3> or -NR<4>R<5>, R<2> represents hydrogen, chlorine, a group of the formula -OR<6> or a group of the formula -NR<7>R<8>, R<3> represents C1-10 alkyl, C3-8 cycloalkyl or aryl-C1-4-alkyl, R<4> represents C1-10 alkyl, C3-8 cycloalkyl, optionally substituted aryl or aryl-C1-4-alkyl, R<5> represents hydrogen, C1-10 alkyl, C3-8 cycloalkyl, optionally substituted aryl or aryl-C1-4-alkyl and R<6> represents C1-10 alkyl, C3-8 cycloalkyl, aryl-C1-4-alkyl or an optionally substituted aromatic or heteroaromatic rest and R<7> and R<8> represent independently C1-10 alkyl, C3-8 cycloalkyl or aryl-C1-4-alkyl or together with the nitrogen atom form a saturated or aromatic heterocyclic ring. The inventive derivatives are obtained by reacting the corresponding 3-chloropyridazines or 3,6-dichloropyridazine with carbon monoxide and alcohols or amines H-R<1> in the presence of palladium-phosphin complexes and bases. The pyridazine carboxylic acid derivatives (Ia, Ib) are the intermediates for the synthesis of pharmaceutically active substances.
专利号:WO-2022000603-A1 优先权日:2020-06-28 标 题 :Synthesis method for pyroxasulfone, and application of pyroxasulfone 发明人:Shen yunhe; ZHU YUCHAO; XIONG GUOYIN 权利人:ANHUI JIUYI AGRICULTURE CO LTD 摘要:The present invention relates to the technical field of pesticides, and provides a synthesis method for pyroxasulfone. The preparation steps comprise: step (1): performing a hydroxylation reaction, a fluoromethylation reaction, and a chlorination reaction on a reactant (I) to obtain an intermediate 2; and step (2): mixing an intermediate 1 with the intermediate 2, adding water to the mixture to separate an organic phase, so as to obtain a transition intermediate, and adding a solvent and an oxidant to the transition intermediate for a reaction to obtain pyroxasulfone. Also provided is an application of pyroxasulfone in pesticides, wherein pyroxasulfone is prepared using the synthesis method. The present invention can not only improve the overall yield of a target product, but also reduce the production of byproducts, thus greatly reducing the production of waste gas, waste water and waste residue and implementing the recycling of a solvent.
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