Preparation method of methyl trifluoropargynate
A technology of methyl trifluoroalkynoate and kung fu acid, which is applied in the field of preparation of methyl trifluoroalkynoate, can solve the problems of low synthesis efficiency, difficulty in synthesizing methyl trifluoroalkynoate, and difficulty in producing seflumethrin, etc. problems, to achieve the effect of waste utilization
Inactive Publication Date: 2019-05-17
江苏春江润田农化有限公司
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Problems solved by technology
However, it is difficult to produce seflumethrin with methyl trifluoroalkynoate as raw material, because the preparation of methyl trifluoroalkynoate is difficult
And the drug effect of methyl methoxy tetrafluorobenzyl alcohol is better than that of tetrafluorobenzyl alcohol, trifluorochrysanthemum acid is better than permethrin, better than the first chrysanthemic acid, so to produce and develop sefluthrin, It is necessary to solve the problems of difficult synthesis and low synthesis efficiency of trifluoroalkynoic acid methyl ester
Method used
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Embodiment 1
[0021] Put 3200kg of mixed solvent of tert-butanol and DMF into a 5000L cyclization kettle, put 380kg of sodium tert-butoxide into it, and quickly add 1000kg of kung fu acid adduct dropwise under the condition of -25°C, and finish the dropwise addition in 60 minutes, and the cyclization reaction obtains Kungfu acid cyclization and trifluoroalkynoic acid methyl ester, the gas spectrum analysis spectrum of the lock solvent normalization method is as follows figure 1 As shown, the content of methyl trifluoroalkynoate is 2.0497%. After desolventizing the reaction solution, the fraction at 80-116°C was collected under the negative pressure condition of -0.098--0.099Mpa, and the crude product of methyl trifluoroalkynoate with a content of 38.2483% was obtained. The CDMC chromatographic analysis diagram is as follows figure 2 shown. Put 2500kg of crude methyl trifluoroalkynoate into a 3000L rectification kettle, pass through a 10-meter-high Ф400 stainless steel column, rectify unde...
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The invention discloses a preparation method of methyl trifluoropargynate. The preparation method includes the steps that 3,3-dimethyl-4,6,6-trichlorine-7,7,7-trifluoroheptanoate and sodium tert-butoxide are cyclized in a mixed solvent of tertiary butanol and N, N-dimethylformamide (DMF) firstly to remove HCl to generate cyclization materials 1R, 3cis-permethrin dichloride and methyl trifluoroparylate. According to the preparation method of the methyl trifluoropargynate, by fine-tuning the temperature of a cyclization process and controlling the distillation pressure and temperature, and on the basis of not increasing the cost of cyclization, the ratio of the methyl trifluoroparylate is increased; and methyl trifluoroparylate crude products with the content being 35-55% are collected through the negative pressure, and then rectified to obtain methyl trifluoroparylate fine products with the content being greater than or equal to 93%, waste utilization during production of lambda cyhalthrin acid is realized, and the requirements of health and pharmaceutical industries are met.
Description
technical field [0001] The invention relates to a method for preparing methyl trifluoroalkynoate, which belongs to the technical field of preparation of pyrethroid intermediates. Background technique [0002] In 2003, the "third-generation" hygienic-thrin technical product - high-efficiency fluorothrin: the advent, application and competition of transfluthrin, perfluthrin and mefluthrin broke the 30-year history The first permethrin series of permethrin products represented by allethrin, ES-bioallethrin (EBT) and dextromethrin (ETOC) are in the leading position in hygienic household medicines, and gradually tetrafluoroethylene The first chrysanthemic acid with Bian Chun as the basic raw material and permethrin with permethrin as the main intermediate take the lead. The efficacy of indoor insecticides with perfluthrin and mefluthrin as the main raw materials is much stronger than that of the first series of permethrin products, and the efficacy of transfluthrin is about 8 t...
Claims
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Login to View More IPC IPC(8): C07C67/30C07C67/54C07C69/747
Inventor 徐永晨张和平张成东钱晖魏康
Owner 江苏春江润田农化有限公司