反应详情

To a stirred slurry of 4,5-dimethoxyisatoic anhydride (4.46 g, 20 mmol) and S-methyl-N-(chloromethanesulfonyl)isothiourea (4.06 g, 20 mmol) in dioxane (30 ml) is added 1,5-diazabicyclo[4.3.0]non-5-ene (2.5 ml). The mixture is refluxed for 4 hr under nitrogen, then cooled and poured into 0.3N aqueous hydrochloric acid. The precipitate is collected by filtration and recrystallized from DMSO to provide the title compound as a light yellow solid, mp >300° C. (445 mg, 7.5%).

1. temperatureThe mixture is refluxed for 4 hr under nitrogen
2. temperaturecooled
3. filtrationThe precipitate is collected by filtration
4. customrecrystallized from DMSO