2524-03-0Relevant articles and documents
-
Lippman,A.E.
, p. 471 - 473 (1966)
-
PROCESS FOR PREPARATION OF O, O-DIMEHYL PHOSPHORAMIDOTHIOATE AND N-(METHOXY-METHYLSULFANYLPHOSPHORYL) ACETAMIDE
-
Paragraph 0032-0033, (2020/02/08)
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.
Synthesis method of O, O-dialkyl thiphosphoryl chloride
-
Paragraph 0040; 0041; 0044-0047, (2018/08/28)
The invention discloses a synthesis method of O, O-diakyl thiphosphoryl chloride. In a reaction system where O, O-dialkyl S-hydro-phophorodithioate and chlorine are subjected to a chlorination reaction to prepare O, O-dialkyl thiphosphoryl chloride, an excess chlorine is introduced to make sulphur generated in the reaction be converted into disulfur dichloride, and disulfur dichloride is convertedinto sulfur dichloride afterwards; and by controlling the reaction temperature and arranging the reaction system to be in the negative pressure state, sulfur dichloride is moved out of the reaction system in the reaction process through distillation and condensing. The synthesis method substantially achieves the atomic economy based on a green chemistry concept; the overall cost of raw materialsis far lower than that in a traditional method, the amount of the three wastes is less, and the three wastes are easy to dispose; a traditional solid-liquid separation step is cancelled, automated production is facilitated, and meanwhile, improvement of the safety and environment production level of the device is facilitated; and O, O-dialkyl thiphosphoryl chloride is not in contact with water, disintegration of the product is avoided, the yield rate is as high as 93%, and the product content can reach 99%.
