In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 513-74-6, name is Ammonium carbamodithioate belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: amides-buliding-blocks
Methyl Dithiocarbamate (I) [2] In a 500mL three-necked flask, provided with a gas-inlet tube, a stirrer, and a gas outlet combined with a thermometer, are placed dry THF(140mL) and carbon disulfide (16.7g, 0.22mol). Ammonia is then introduced with continuous stirring, the flow of ammonia being adjusted in such a way that a slow stream is leaving the flask. The temperature is allowed to rise to 40-45 °C and is kept at that level by occasional cooling. When, after 1h, no more heat is evolved and the temperature has dropped to 35 °C, the flask is evacuated (rotary evaporator) to remove some dissolved ammonia. Water (25mL) is then added to dissolved the white precipitate. To the resultant mixture of THF and aqueous ammonium dithiocarbamate, dimethylsulfate (25.2g, 0.2mol) is added with vigorous stirring. During the addition (which requires 30min), the temperature of the mixture is allowed to rise to 45-50 °C and is maintained at that level for 15 min by occasional cooling. Then, concentrated aqucous ammonia (5mL) is added to destroy excess dimethyl sulfate and stirring is continued for 15min. The upper layer is separated and dried with magnesium sulfate (without being washed). The aqueous layer is extracted with EA (3*20mL) and the organic phases are combined. The solution is concentrated in a water-pump vacuum and the last traces of solvent are removed at 0.5-1 torr by means of an oil pump to leave nearly pure methyl dithiocarbamate(I); yield: 20g (93percent, calculated on dimethyl sulfate).
The synthetic route of 513-74-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Shin Nippon Biomedical Laboratories, Ltd.; SUZUKI, Nobuyuki; YAMASHITA, Hidetoshi; (156 pag.)EP3018125; (2016); A1;,
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