Oriental (Luzhou) Agrochemicals Co., Ltd.

Zhejiang Zhuji United Chemicals Co., Ltd.

Other

Max (Rudong) Chemicals Co., Ltd.

Oriental Agrochemicals. Co., Ltd.

Bangchi Chen

Zhongyuan Wang

Yinwei Sun

Qiuju Sheng

Tianhao Zhang

Baochuan Guan

Jinlong Zhang

Junliang Wang

Hao Jiang

Pan Zhang

Zhiming Zhang

Xiaomin Liang

Junjin Zhou

Jinzhi Yang

Haige Teng

Jieping Shi

Tao Jin

Xiaohua Yu

Xiaoyan Xu

Guoping Cai

Yehua Su

Zhuoya Zhang

Haiping Mu

Miao Lin

Yonglin Zhang

Hongwei Zhang

Xianbo Xu

Jianxin Lu

Yanyan Huang

Xiaodong Du

Teng Lai

Zhenghe Yang

The application provides a high-purity thermostable crystal form of a substituted 3-isoxazolidinone compound, a preparation method therefor and an application thereof. The High-purity thermostable crystal form is prepared by a particular method of the present technology and is determined by single-crystal X-ray diffraction as an orthorhombic crystal, featuring a space group of P212121 and lattice parameters of a=9.2301(2) Å, b=11.0751(3) Å, c=12.7554(3) A, α=90°, β=90°, and γ=90°. The orthorhombic crystal can be conveniently applied in preparation of agrochemical formulations, such as a suspension concentrate and a water dispersible granule, and the new formulations prepared have a better herbicidal activity and crop safety.

High-purity thermostable crystal form of substituted 3-isoxazolidinone compound, preparation method therefor and application thereof

Disclosed are a type of conjugated triene compounds (1), and a preparation and application thereof. In this method, a 2-(cyclohexenylidene)malonic acid derivative is sequentially subjected to isomerization, halogenation reaction in the presence of a halogenating agent and dehydrohalogenation to prepare the conjugated triene compounds (1). This disclosure further provides a method of preparing a 2-aryl malonic acid derivative from the conjugated triene compounds (1) through aromatization reaction.

Conjugated triene compound, and preparation and application thereof

Disclosed herein is a method for preparing a 2-arylmalonic acid derivative. In this method, a cyclohexadiene compound is used as a raw material, and sequentially undergoes an isomerization reaction, a halogenation reaction in the presence of a halogenating agent and a dehydrohalogenation-aromatization reaction to obtain a 2-arylmalonic acid derivative (3). An intermediate for preparing the 2-arylmalonic acid derivative (3) and use of the intermediate are also disclosed.

Method for preparing 2-arylmalonic acid derivative and intermediate, and use thereof

Disclosed are a type of halogenated conjugated diene compounds (1), and preparation and application thereof. In this method, a conjugated diene compounds is subjected to halogenation reaction to prepare the compound (1). This disclosure further provides a method of preparing a 2-arylmalonic acid derivative from the compound (1) through dehydrohalogenation and aromatization reaction. 

Halogenated conjugated diene compound, and preparation and application thereof

Disclosed herein are a preparation method and an application of an isoxazinone compound (I), where the preparation method includes: reacting compound (II) with a carboxylic acid (III) in the presence of a dehydrating agent and a base to produce the isoxazinone compound (I); and subjecting the isoxazinone compound (I) and a protonic acid salt of an amino compound (IV) or ROH (VII) to ring-opening reaction in the presence of a base to produce a bisamide compound (V) or an N-acyl benzoate compound (VI).

Preparation method and application of isoxazinone compounds

Disclosed are a method for preparing 2-(cyclohexenylidene) malonic acid derivatives and uses thereof. In this method, an olefin and a 2-substituted malonic acid derivative are used as starting materials to prepare the 2-(cyclohexenylidene) malonic acid derivative in the presence of a catalyst through cyclization reaction. This method has the following advantages: (1) the method can be very efficiently used for the synthesis of highly sterically-hindered 2-(2,6-disubstituted cyclohexenylidene) malonic acid derivatives; (2) the reaction yield is high, the reaction conditions are mild, and the wastes are less, favorable for industrial production. More importantly, the present invention extends the further use of 2-(cyclohexenylidene)malonic acid derivatives in organic synthesis, especially in the synthesis of 2-aryl malonic acid derivatives and their corresponding drugs such as Pinoxaden.

Method for preparing 2-(cyclohexenylidene) malonic acid derivatives and uses thereof

Disclosed herein is a method of preparing N-acyl anthranilamide (I), including: reacting a substituted anthranilic acid (II) with pyrazolecarboxylic acid (III) under the action of a phosphorus reagent and a base to obtain an intermediate benzoxazinone (IV); and subjecting the intermediate benzoxazinone (IV) and a protonic acid salt of methylamine to a ring-opening reaction to obtain N-acyl anthranilamide (I), as shown in the following reaction scheme: 

Method of preparing N-acyl anthranilamide

Disclosed is a method of synthesizing 1,2,4-triazole-3-thione compounds and intermediates thereof. The method includes reacting a hydrazine with glyoxylic acid to form a hydrazono acetic acid intermediate followed by reacting the latter with thiocyanate to obtain the 1,2,4-triazole-3-thione compound. The raw materials involved in the present method are readily available, and the reaction is very specific in terms of regioselectivity, resulting in minimum by-product and high product yield. There are neither specific requirements for special equipment nor special operations such as high vacuum, high temperature, anhydrous and oxygen-free manipulations. The process is simple and generates minimum wastes, suitable for industrial production.

Method of synthesizing l,2,4-triazole-3-thione compounds and intermediates thereof

Disclosed are a method for preparing 2-aryl malonamide and an application thereof. This method uses 2-(cyclohexenylidene) malononitrile as a raw material, which undergoes an aromatization-hydrolyzation reaction in the presence of an oxidant and water to produce 2-aryl malonamide by one step. Compared to the prior art, the method for preparing 2-aryl malonamide of this application has the following features and advantages: (1) this method employs a completely different synthetic strategy; (2) raw materials used in this method are easily obtained; (3) this method not only has high yield, but also does not require expensive metal catalysts. This method is lower-cost, suitable for the industrial production.

Method for preparing 2-aryl malonamide and applications thereof

Disclosed are a method of synthesizing prothioconazole and optically active isomers thereof and intermediates. The method includes reacting hydrazine with glyoxylic acid to produce a hydrazono acetic acid as an intermediate, and then reacting the intermediate with thiocyanate to produce the target product prothioconazole. The present method is very specific in terms of regioselectivity, resulting in minimum byproducts and a high product yield. The present method does not require special equipment, nor anhydrous or oxygen-free manipulations. The process is simple and generates minimum wastes, suitable for industrial production.

Method of synthesizing prothioconazole and optically active isomers thereof and intermediates

The present invention discloses a sulfonamide compound (III) which is intermediately produced in a process for preparing a high-purity sulfonamide compound (I). The preparation comprises the following steps: a, taking a crude product of a sulfonamide compound (I) as an initial raw material, and enabling the raw material to react with a compound of a formula (II) in presence of alkali and a catalyst so as to synthesize an intermediate of a formula (III); and b, enabling the compound represented by the formula (III) to react with alkali or acid, thereby obtaining the high-purity sulfonamide compound (I).

Intermediate of preparing high-purity sulfonamide compound

A preparative method for carboxylic acids is disclosed in the present invention. The method is characterized in that: compounds (II) are reacted in the presence of hydrogen peroxide and base to produce target products (I), as represented by the following reaction scheme: wherein Ris aryl, pyridyl, pyrimidyl, pyridazinyl, pyrazinyl, benzothienyl, benzofuranyl, quinolinyl, isoquinolinyl, thiadiazolyl, Calkyl, Ccycloalkyl, Calkenyl, Calkynyl and hydrogen; Ris alkoxycarbonyl, alkylaminocarbonyl, aminocarbonyl, alkylthiolcarbonyl, cyano, sulfonyl, sulfinyl, carbonyl, aldehyde, carboxyl, nitro, alkyl and hydrogen; Ris alkoxycarbonyl, alkyl amido carbonyl, aminocarbonyl, cyano, sulfonyl, sulfinyl, carbonyl, carboxyl and nitro. The present invention has the following main benefits: cheap and readily available starting materials, safe processes, high yield, good quality, which facilitates industrial production.

Preparative method for carboxylic acids

The present invention discloses a method for preparing a high-purity sulfonamide compound and an intermediate of the sulfonamide compound. The method comprises the following steps: a, taking a crude product of a sulfonamide compound (I) as an initial raw material, and enabling the raw material to react with a compound of a formula (II) in presence of alkali and a catalyst so as to synthesize an intermediate of a formula (III); and b, enabling the compound represented by the formula (III) to react with alkali or acid, thereby obtaining the high-purity sulfonamide compound (I).

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Zhejiang, China

Bangchi Chen