3260-88-6Relevant articles and documents
Preparation method of 6-chloro-2-methoxytoluene and synthesis process of methoxyfenozide
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Paragraph 0046; 0052-0054, (2021/08/14)
The invention relates to the field of insecticides, in particular to a preparation method of 6-chloro-2-methoxytoluene and a synthesis process of methoxyfenozide. The preparation method of the 6-chloro-2-methoxytoluene comprises the following steps: in a solvent, mixing 2, 6-dichlorotoluene with sodium methoxide, and carrying out a substitution reaction to prepare a first reaction solution containing 3-chloro-2-sodium methylphenolate and the 6-chloro-2-methoxytoluene; and dropwise adding dimethyl sulfate into the first reaction solution, carrying out etherification reaction, removing 3-chloro-2-sodium methylphenolate to obtain a second reaction solution, and carrying out post-treatment to obtain the 6-chloro-2-methoxytoluene. The synthesis process of the methoxyfenozide comprises the following steps: preparing 3-methoxy-2-methyl benzoic acid by taking 6-chloro-2-methoxytoluene as an intermediate; using 3-methoxy-2-methyl benzoic acid and 3, 5-dimethyl benzoic acid as intermediates, and preparing to obtain the methoxyfenozide. According to the synthesis process disclosed by the invention, the yield and the purity of methoxyfenozide can be remarkably improved.
Preparation method of 2-methyl-3-methoxybenzoic acid
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Paragraph 0018; 0020, (2018/03/24)
The invention relates to a preparation method of 2-methyl-3-methoxybenzoic acid. The preparation method comprises the following specific steps: A, adding a proper amount of a sodium methoxide solution, 2,6-dichlorotoluene, dimethylformamide and cuprous salt into a reaction kettle; stirring and raising the temperature; controlling the temperature to 80 DEG C to 150 DEG C and reacting to obtain 2-methyl-3-chloroanisole; B, adding a proper amount of tetrahydrofuran and magnesium into the other reaction kettle; controlling the temperature to be 30 DEG C to 60 DEG C; adding a mixed solution of bromoethane and the 2-methyl-3-chloroanisole; after reacting for 20min to 40min, controlling the temperature to be 40 DEG C to 60 DEG C and dropwise adding the 2-methyl-3-chloroanisole; after dropwise adding, keeping heat and reacting for 1.5h to 2.5h; then cooling to -15 DEG C to -5 DEG C; adding dry ice by batches; controlling the temperature to be 0 DEG C to 20 DEG C, keeping the heat and reactingfor 2h to 4h; then recycling the tetrahydrofuran; adjusting the pH (Potential of Hydrogen) value to separate out white powder, namely the 2-methyl-3-methoxybenzoic acid. The preparation method of the2-methyl-3-methoxybenzoic acid, provided by the invention, is simple in route and high in yield.
Method for synthesizing 6-chloro-2-methoxytoluene
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Paragraph 0025; 0026; 0027; 0028; 0029; 0030-0049, (2017/06/02)
The invention discloses a method for synthesizing 6-chloro-2-methoxytoluene. The method comprises the following steps: dissolving 2,6-dichlorotoluene in an aprotic polar solvent, dripping sodium methylate for reacting, maintaining the temperature to be 40-170 DEG C after dripping completion, and performing a reaction for 2-20 hours; reducing the temperature to be 20-120 DEG C after temperature maintaining is completed; adding a phase transfer catalyst into the reaction solution, introducing a chloromethane gas for reacting until the mass fraction of 6-chloro-2-hydroxy methylbenzene in the reaction solution is less than 1%, and maintaining the temperature and performing a reaction for 0.1-2 hours; performing cooling to room temperature after the reaction; and recovering the aprotic polar solvent under negative pressure, performing after-treatment, thereby obtaining the 6-chloro-2-methoxytoluene. According to the method, the 6-chloro-2-methoxytoluene is synthesized by chloromethane, the reaction speed of the chloromethane is improved by using a small amount of catalysts in the method, and the chloromethane can serve as a methylation reagent under normal pressure; and moreover, the yield of the 6-chloro-2-methoxytoluene is greater than 93%, and the method disclosed by the invention is easy to operate, low in cost and slight in environmental hazards.