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公开(公告)号：US20210321613A1
公开(公告)日：2021-10-21
申请号：US17251005
申请日：2019-06-12
IPC分类号： A01N43/32 , C07D341/00
摘要： A process for preparation of thiocyclam base and salt. A method of manufacturing N,N-dimethyl-1,2,3-trithian-5-ylainine hydrochloride is described including the steps of: providing a mixture of thiosulfuric acid S, S′[2-(dimethylamino) trimethylene] ester monosodium salt and sodium hydroxide; adding an aqueous saline solution to the mixture of thiosulfuric acid S, S′-[2-(dimethylamino) trimethylene] ester monosodium salt and sodium hydroxide; separating the phases of the mixture; collecting the solids from the mixture using filtration; washing the solids with organic solvent; and drying the solids, where the dried solids are methyl-1,2,3-trithian-5-ylamine hydrochloride, and where the yield of the N,N-dimethyl-1,2,3-trithian-5-ylamine hydrochloride is increased by incorporation of a body charge of diatomaceous earth into the saline addition step, forming a mixture of the diatomaceous C earth with the composition of this step, and filtering the charged mixture through a diatomaceous earth media prior to the separation step.
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公开(公告)号：US11198700B2
公开(公告)日：2021-12-14
申请号：US16860182
申请日：2020-04-28
发明人： Vic Prasad , David Huang , Kamal Kataria , Christopher Lynn Larson , Cameron Seath Gibb , Stephen Cornes
摘要： Preparation of O,O-dimethyl phosphoramidothioate and O,O-dimethyl phosphoroamidothioate. A process of making O,O-dimethyl phosphoroamidothioate is described including reacting sulfur with PCl3 to form PSCl3, reacting the PSCl3 formed with methanol to form O-methyl phosphorodichloridothioate, and reacting the O-methyl phosphorodichloridothioate formed with methyl lye to form O,O-dimethyl phosphorochloridothioate in solution in CH2Cl2, and reacting the O,O-dimethyl phosphorochloridothioate formed with sodium hydroxide and ammonium hydroxide to form O,O-dimethyl phosphoroamidothioate in solution in CH2Cl2. Reacting the O,O-dimethyl phosphoroamidothioate formed with catalytic dimethyl sulfate to form methamidophos and reacting the methamidophos formed with acetic anhydride to form N-(methoxy-methylsulfanylphosphoryl) acetamide is also described. Throughout the process, the O,O-dimethyl phosphorochloridothioate and the O,O-dimethyl phosphoroamidothioate formed are maintained in solution in CH2Cl2 at all times.
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公开(公告)号：US11708322B2
公开(公告)日：2023-07-25
申请号：US16685703
申请日：2019-11-15
发明人： Kamal Kataria , Vic Prasad , Christopher Lynn Larson , Cameron Seath Gibb , Kirit Desai , Ashwani Gupta , Girish Sisode
IPC分类号： C07C253/30
CPC分类号： C07C253/30
摘要： Disclosed herein a process preparation of 2,6-dichlorobenzonitrile. A process of making high yield, high purity 2,6-dichlorobenzonitrile including the selective de-nitrochlorination of 2-chloro-6-nitrobenzonitrile by treatment of the 2-chloro-6-nitrobenzonitrile with chlorine gas.
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4.发明授权公开(公告)号：US10669295B2
公开(公告)日：2020-06-02
申请号：US16040136
申请日：2018-07-19
发明人： Vic Prasad , David Huang , Kamal Kataria , Christopher Lynn Larson , Cameron Seath Gibb , Stephen Cornes
摘要： Preparation of O,O-dimethyl phosphoramidothioate and O,O-dimethyl phosphoroamidothioate. A process of making O,O-dimethyl phosphoroamidothioate is described including reacting sulfur with PCl3 to form PSCl3, reacting the PSCl3 formed with methanol to form O-methyl phosphorodichloridothioate, and reacting the O-methyl phosphorodichloridothioate formed with methyl lye to form O,O-dimethyl phosphorochloridothioate in solution in CH2Cl2, and reacting the O,O-dimethyl phosphorochloridothioate formed with sodium hydroxide and ammonium hydroxide to form O,O-dimethyl phosphoroamidothioate in solution in CH2Cl2. Reacting the O,O-dimethyl phosphoroamidothioate formed with catalytic dimethyl sulfate to form methamidophos, and reacting the methamidophos formed with acetic anhydride to form N-(methoxy-methylsulfanylphosphoryl) acetamide is also described. Throughout the process, the O,O-dimethyl phosphorochloridothioate and the O,O-dimethyl phosphoroamidothioate formed are maintained in solution in CH2Cl2 at all times.
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