反应详情

Hydrogen sulfide (gas) was bubbled into a solution of (3,4-dichloro-phenyl)-acetonitrile (1.86 g, 10 mmol, 1.0 eq)) and triethyl amine (10 mmol, 1 eq) in ethanol (10 ml) for about 1 hour. After 1 hour the reaction mixture capped and stirred at room temperature overnight. TLC showed that most of nitrile was converted to thioacteamide. Excess of H2S was removed by bubbling nitrogen into the reaction mixture for 30 min. The reaction mixture was then concentrated and purified by silica gel chromatography (ISCO system, 30–60% ethylacetate/hexane) to give the title compound (1213) (55% yield).

1. customAfter 1 hour the reaction mixture capped
2. customExcess of H2S was removed
3. customby bubbling nitrogen into the reaction mixture for 30 min
4. concentrationThe reaction mixture was then concentrated
5. custompurified by silica gel chromatography (ISCO system, 30–60% ethylacetate/hexane)