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ChemicalBook CAS DataBase List Dimethylphosphorodithioate

Dimethylphosphorodithioate synthesis

8synthesis methods
-

Yield:756-80-9 97%

Reaction Conditions:

with pyridine;dmap;tetraphosphorus decasulfide;dimethylsulfide at 25 - 55; under 40 Torr; for 1 h;Large scale;Pressure;Temperature;

Steps:

4.1; 4.2; 4.3
(1) Add 1500 kg of methyl sulfide mother liquor to the reactor, add 1000 kg of phosphorus pentasulfide to the reactor, stir for 0.5 h, and beaten for 1 h.Making the phosphorus pentasulfide and methyl sulfide mother liquor into a slurry to obtain a reaction liquid A;(2) taking 1kg of DMAP and 1kg of pyridine mixed as a catalyst, added to 582kg of methanol and mixed to obtain a reaction solution B;(3) controlling the pressure condition of the reaction vessel to a vacuum of 40 mmHg, and heating the reaction liquid A in the reaction vessel to 25 ° C, and starting to dropwise add the reaction liquid B to the reaction vessel; After the completion of the dropwise addition, the reactor is heated to 55 ° C for 1 h, and the hydrogen sulfide gas generated by the reaction is continuously extracted by the micro-negative pressure during the reaction, and the hydrogen sulfide gas is absorbed by the alkali solution. After the reaction is completed, The desired O,O-dimethyldithiophosphate is obtained. The content of O,O-dimethyldithiophosphate in the reaction was calculated to be 98%, and the calculated product yield was 97%.

References:

Texas Lvba Fine Chemical Co., Ltd.;Tian Junjie;Sun Zaichen;Zhang Xuezhong;Zhang Jinwang CN108864181, 2018, A Location in patent:Paragraph 0023; 0029; 0035; 0037; 0039-0042; 0044; 0047

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