sodium O,O-dimethyl thiophosphate synthesis
- Product Name:sodium O,O-dimethyl thiophosphate
- CAS Number:23754-87-2
- Molecular formula:C2H6NaO3PS
- Molecular Weight:164.0958
868-85-9
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Yield:23754-87-2 96.31%
Reaction Conditions:
Stage #1:Dimethyl phosphite with sodium in methanol at 40; for 0.333333 h;
Stage #2: with sulfur in methanol at 50; for 5 h;
Steps:
1.2; 2.2; 3.2; 4.2; 5.2; 6.2; 7.2; 8.2 (2) Preparation of sodium O, O-dimethylthiophosphate
9.28 g (0.4 mol) of sodium metal was added in portions to 150 mL of anhydrous methanol. After the addition was completed, 44 g (0.4 mol) of a dimethyl phosphite solution in methanol (30 mL) was added dropwise after the temperature was lowered to 40 ° C, and the reaction was carried out for 20 minutes after the completion of the dropwise addition. 12.8 g (0.4 mol) of sulfur powder was added in portions, and the reaction was carried out at 50 ° C for 5 hours after the addition. After naturally dropping to room temperature, the unreacted sulfur is removed by filtration. The solvent was removed by rotary evaporation to obtain a white solid of O,O-dimethyl thiophosphate.Wash once with water and acetone in a volume ratio of 1:5. Dry at 60 ° C for 10 hours under vacuum. Obtained 63.22 g of white needle crystal O,O-dimethylthiophosphate, yield 96.31%;
References:
Henan Chemical Institute Co., Ltd.;Huo Erfu;Cheng Weiqin;Feng Ming;Wang Bonan;Wang Yanhua;Chang Shuhao;Dong Guangxia;Yang Shuai;Wang Yinan CN109651432, 2019, A Location in patent:Paragraph 0114; 0117; 0118
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23754-87-2
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2636-26-2
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