ChemicalBook CAS DataBase List Dithiobiuret

Dithiobiuret synthesis

5synthesis methods

Product Name:Dithiobiuret
CAS Number:541-53-7
Molecular formula:C2H5N3S2
Molecular Weight:135.21

N,N-Dimethylthiocarbamoyl Isothiocyanate

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Yield:-

Reaction Conditions:

with sodium hydroxide in chloroform;acetone

Steps:

5 Preparation of the hydrobromic acid salt of 3-dimethylamino-5-[N-(2-dimethylaminoethyl)-N-methylamino]-1,2,4-dithiazolium bromide
EXAMPLE 5 Preparation of the hydrobromic acid salt of 3-dimethylamino-5-[N-(2-dimethylaminoethyl)-N-methylamino]-1,2,4-dithiazolium bromide A solution of 10.2 parts of N,N,N'-trimethylethylenediamine in 20 parts of acetone was added dropwise to a solution of 14.2 parts of dimethylthiocarbamoyl isothiocyanate in 100 parts of acetone at 10°-15° C. The resulting solution was allowed to warm to room temperature and stirred for 2 hours. This solution was then filtered and evaporated under reduced pressure. The residue was added to 50 parts of a 10% sodium hydroxide solution. This solution was washed with 100 parts of chloroform, neutralized with glacial acetic acid, and then extracted twice with 50 parts of methylene chloride. The combined methylene chloride extracts were dried, filtered, and evaporated under reduced pressure to give 13 parts of the crude dithiobiuret product. This product was then recrystallized from ethanol to afford 5 parts of the required dithiobiuret, m.p. 93°-94° C. 5 Parts of this dithiobiuret were dissolved in 30 parts of methanol at 10° C.

References:

E. I. Du Pont de Nemours and Company US3944670, 1976, A

21867-64-1 Synthesis