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ChemicalBook CAS DataBase List N-Cyanoimido-S,S-dimethyl-dithiocarbonate

N-Cyanoimido-S,S-dimethyl-dithiocarbonate synthesis

9synthesis methods
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Yield:10191-60-3 93%

Reaction Conditions:

Stage #1:CYANAMID with potassium hydroxide in acetone for 0.25 h;
Stage #2:carbon disulfide in acetone at 10 - 15; for 2 h;
Stage #3:dimethyl sulfate at 40 - 45; for 6 h;

Steps:

1 Example 1
Add 40percent potassium hydroxide solution (70 g, 0.5 mol) to a mixed solution of 75 ml acetone and 30percent amine cyanide (35 g, 0.25 mol) while stirring.The addition is completed in 15 minutes.The temperature of the reaction system was reduced to 10-15°C, carbon disulfide (19.5 g, 0.254 mol) was added, and the temperature was maintained at 10-15°C for 2 hours.Raise the temperature to 2025, stand for layering, recover the organic layer, and heat the water layer to 4045,Dimethyl sulfate (64 g, 0.5 mol) was added dropwise to the water layer, and the addition was completed in 1 hour.The reaction mixture is heated to reflux for 5 hours, then the temperature is lowered to 5-10°C, and the temperature is maintained for 0.5 hours.The precipitate separated out, filtered, and dried to obtain 33.9 g of light yellow intermediate II with a yield of 93percent.

References:

Qingdao Agricultural University;Li Yuwen;Ma Cuili CN111440127, 2020, A Location in patent:Paragraph 0007

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