Dimethylamine → HCID 13720654, compound

Participants

Reaction Conditions

Reaction Steps

A solution of methyl 2-(pyrid-2-yl)tetrahydrothiophene-2-carbodithioate (20 g) in dimethylamine (100 cc) is heated gradually for 3 hours 40 minutes, in an autoclave, up to a temperature of about 125° C. After cooling to a temperature of about 20° C., the autoclave is emptied and rinsed with methylene chloride (200 cc), the latter being added to the reaction mixture. The solution is concentrated to dryness (20 mm Hg; 2.7 kPa) at 40° C. The resulting residue (20.7 g) is dissolved in boiling ethanol (50 cc) and the solution, to which decolourising charcoal (0.5 g) is added, is filtered hot and then kept, after cooling, for 1 hour at a temperature of about 0° C. The crystals which have appeared are filtered off, washed twice with ethanol (20 cc in total) and dried under reduced pressure (20 mm Hg; 2.7 kPa) at a temperature of about 20° C. The resulting product (14.1 g) is dissolved in boiling ethanol (45 cc) and the solution, to which decolourising charcoal (0.5 g) is added, is filtered hot and then kept, after cooling, for 1 hour at a temperature of 0° C. The crystals which have appeared are filtered off, washed twice with ethanol (20 cc in total) and dried under reduced pressure (1 mm Hg; 0.13 kPa) at 45° C. N,N-Dimethyl-2-(pyrid-2-yl)-tetrahydrothiophene-2-carbothioamide (11.8 g), melting at 100° C., is thus obtained.

Provenance & Evidence