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A kind of preparation method of pyrimidine salicylic acid herbicide pyrimidine saflufenacil
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A technology of pyrimidine salicylic acid and pyrimidine saflufenacil, which is applied in the field of agrochemicals and achieves the effects of high yield, good purity and mild reaction
Active Publication Date: 2016-06-08
台州煜农生物科技有限公司
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This patent is based on the original patent, using the herbicide bispyribac as the starting material, through a one-step method to prepare the safe and efficient broad-spectrum pyrimidine salicylic acid herbicide pyrimidine saflufenacil, that is, using bispyribac as the raw material under the action of the catalyst Dehydrationcondensation reaction with benzophenone oxime to prepare saflufenacil in one step, which solved the complex process problem of multi-step preparation of saflufenacil in LG Chemical Company
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example 1
[0021] Example 1: Preparation of pyrimidine saflufenacil
[0022] Add bispyribac (43.0g, 100mmol), benzophenone oxime (20.8g, 107mmol), DCC (22.5g, 107mmol), DMAP (1.25g, 10mmol), 500ml of dichloromethane into a 1L reaction flask, Under the protection of nitrogen, react at room temperature for 20 hours. After the reaction results, filter, and the filtrate is concentrated under reduced pressure to recover dichloromethane to obtain saflufenacil product, which is then recrystallized with toluene to obtain saflufenacil in white crystals (56.01 g, 91.9%), melting point: 128.5~130.5℃, purity 98.2%, 1 HNMR (CDCl3, 300MHz): δ: 7.10-7.50 (m, 13H), 5.75 (s, 2H), 3.78 (s, 12H).
example 2
[0023] Example 2: Preparation of pyrimidine saflufenacil
[0024] Add bispyribac (43.0g, 100mmol), benzophenone oxime (19.5g, 100mmol), DIC (12.6g, 100mmol), HOBt (1.62g, 12mmol), 1,2-dichloro 395 milliliters of ethane, under the protection of nitrogen, reacted at room temperature for 24 hours, after the reaction results, filtered, and the filtrate was concentrated under reduced pressure to recover 1,2-dichloroethane to obtain the saflufenacil product, which was then reconstituted with tolueneCrystallization gave saflufenacil (55.1 g, 90.4%) as white crystals.
example 3
[0025] Example 3: Preparation of pyrimidine saflufenacil
[0026] Add bispyribac ether (43.0g, 100mmol), benzophenone oxime (29.1g, 150mmol), EDCI (23.3g, 150mmol), 4-PPY (2.53g, 30mmol), 1,2 - 788 milliliters of dichloroethane, under the protection of nitrogen, react at room temperature for 18 hours, after the reaction results, filter, and the filtrate is concentrated under reduced pressure to recover 1,2-dichloroethane to obtain the saflufenacil product, which is then used Recrystallization from toluene gave saflufenacil (55.3 g, 90.7%) as white crystals.
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Abstract
The invention discloses a preparation method of pyribenzoxim belonging to pyrimidinylthiobenzoate herbicide and belongs to the field of agricultural chemistry. The method is carried out as following: taking another pyrimidinylthiobenzoate herbicide-bispyribac sodium salt as a raw material, adding the bispyribac sodium salt, an organic solvent, an alkaline catalyst, a dehydrating agent and diphenyl ketoneoxime into a reaction bulb, letting them react for 6-36 hours under a common temperature, tracking the reaction with TLC, filtering the resultant after the reaction, steaming, removing and recovering the organic solvent from the filtrate under decompression and then carrying out recrystallization with methylbenzene to obtain the pyribenzoxim herbicide of a white solid shape. The invention provides a preparation method of the pyribenzoxim-the pyrimidinylthiobenzoate herbicide which is safe and has a broad spectrum through a dehydration reaction of the raw materials of the pyribenzoxim-the pyrimidinylthiobenzoate herbicide and the diphenyl ketoneoxime with the efficient acylation catalyst and the condensing agent. The preparation process is high in yield (over 90.4%). The technique is a green and clean process technique for production and applicable to mass preparation of the safe and efficient broad-spectrum pyribenzoxim-the pyrimidinylthiobenzoate herbicide.
Description
technical field [0001] The present invention relates to a safe and high-efficiency broad-spectrum paddy fieldpyrimidinesalicylic acid herbicide --- a preparation method of pyribenzoxim (Pyribenzoxim), in particular to a pyrimidinesalicylic acid herbicide bispyribac (Bispyribac) The method for preparing pyrimidinesaflufenacil with benzophenoneoxime in a one-step method as a raw material belongs to the field of agricultural chemistry. Background technique [0002] Pyrimidinesalicylic acid herbicides are another class of acetolactate synthase (ALS) inhibitors successfully developed in the 1990s, which can control a variety of intractable weeds. Spectrum, high selectivity and environmental friendliness have received great attention. It is researched and developed on the basis of the structure optimization of sulfonylurea herbicides. Its herbicidal spectrum and activity are superior to those of sulfonylurea herbicides. Disadvantages such as drug damage. At present, the m...
Claims
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