反应详情

A solution of sodium methoxide (25% wt/v in methanol, 190 mL, 880 mmol) was added dropwise to a stirred suspension of 2,3,6,7-tetrachloroquinoxaline (106 g, 400 mmol) in methanol (1400 mL) at room temperature under nitrogen. After 3 days, a solution of sodium methoxide (25% wt/v in methanol, 40 mL, 190 mmol) was added, followed by tetrahydrofuran (300 mL). The reaction mixture was heated under reflux for 5 minutes, cooled, concentrated to a small volume under reduced pressure and poured into water (500 mL). The precipitate was collected by filtration and washed with water to afford the title compound (97 g, 95%) as a pink solid, mp 144-146° C.

1. temperatureThe reaction mixture was heated
2. temperatureunder reflux for 5 minutes
3. temperaturecooled
4. concentrationconcentrated to a small volume under reduced pressure
5. additionpoured into water (500 mL)
6. filtrationThe precipitate was collected by filtration
7. washwashed with water