反应详情

To a stirred slurry of 4-chloroisatoic anhydride (4.95 g, 25 mmol) and S-methyl-N-(chloromethanesulfonyl)isothiourea (5.07 g, 25 mmol) in acetonitrile (25 ml) under nitrogen is added 4-(N,N-dimethylamino)pyridine (3.97 g, 33 mmol). The mixture is refluxed under nitrogen for 24 hr, concentrated, then worked up as in Example 4 above. The resulting gummy solid is triturated with hot ethanol, then recrystallized from DMF to provide the title compound as a white solid, mp >300° C. (1.65 g, 24%)

1. temperatureThe mixture is refluxed under nitrogen for 24 hr
2. concentrationconcentrated
3. customThe resulting gummy solid is triturated with hot ethanol
4. customrecrystallized from DMF