Electric Literature of 513-74-6, These common heterocyclic compound, 513-74-6, name is Ammonium carbamodithioate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
General procedure: Following literature procedures,1 ammonia gas was bubbled into carbon disulfide 1 (16.7g, 0.22 mol) in THF (100 ml) keeping the temperature below 45 ¡ãC. After 1 hr, the reaction was stopped by allowing the temperature to decrease to rt. The excess ammonia gas was removed by streaming N2 for 30 min or by rotary evaporation under vacuum. The precipitate was collected by filtration to afford white solid ammonium dithiocarbamate 2 (23.1 g, 96percent). Methyl iodide (17.8 g, 0.125 mol) was added to a solution of 2 (5.5 g, 0.05 mol) in acetone (100 ml) at rt and the mixture was stirred for 24 hr. The solid was collected by filtration, washed with chilled acetone (20 ml) and dried under vacuum to provide white solid S,S?-dimethyliminodithiocarbonate hydroiodide ammonium iodide 3 (18.9 g, 96percent). 3 (7.9 g, 0.02 mol) was treated with sat. aq. NaHCO3 solution (100 ml x 2) and the organic products extracted with dichloromethane (50 ml). The organic layer was dried over Na2SO4 and concentrated in vacuo to a clear, colorless liquid 4 (2.3 g, 95percent). 1H NMR (400 MHz, CDCl3) delta 8.88 (s, 1H), 2.42 (s, 6H). 13C NMR (101 MHz, CDCl3) delta 172.10, 14.50. HRMS (ESI+) m/z calcd for C3H8N+ 122.0098, found 122.0096.
Statistics shows that Ammonium carbamodithioate is playing an increasingly important role. we look forward to future research findings about 513-74-6.
Reference:
Article; Pollock, Julie A.; Kim, Sung Hoon; Katzenellenbogen, John A.; Tetrahedron Letters; vol. 56; 44; (2015); p. 6097 – 6099;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics