反应详情

To a solution of dimethyl cyanodithioiminocarbonate (2.85 g, 17.6 mmol) in methanol (20 mL) was added ethylamine (2M soln, 9.7 mL, 19.4 mmol). The solution was allowed to stir at reflux overnight. The solution was cooled to room temperature and the desired product crystallized out of solution over 2 hours. The crystals were collected on a buchner funnel, washed with cold methanol several times, and dried in vacuo to give 1-ethyl-2-methyl-3-cyanoisothiourea as a white solid (1.08 g, 43%). 1H NMR (CDCl3) δ 1.22 (t, 3H, J=6 Hz), 2.61 (s, 3H), 3.35 (s, 1H), 3.46 (q, 2H, J=6 Hz).

1. temperatureat reflux overnight
2. customthe desired product crystallized out of solution over 2 hours
3. customThe crystals were collected on a buchner funnel
4. washwashed with cold methanol several times
5. customdried in vacuo