反应详情

6,8-Dichloro-2-anilino-2,3,4,9-tetrahydro-1H-pyrrolo[3,4-b]quinoline-1,3,9-trione (0.60 g, 1.60 mM) was stirred in methanol (200 mL) and methanesulfonic acid (20 mL) was added with cooling, maintaining the temperature below 20° C. The resulting orange solution was stirred overnight at room temperature. A precipitate formed overnight and the orange suspension was heated to reflux for 1 hour. The suspension was cooled to room temperature and allowed to stand overnight without stirring. The suspension was filtered and the filtrates were slowly diluted with water (200 mL) to give a yellow suspension. This suspension was stirred for two hours and the solids were collected and washed with water, aqueous methanol, 50% methanol/ether, and ether to give the title compound (0.368 g, 61%) as a light tan powder, mp 361-363° C.; MS(CI): 374 (M+H).

1. temperaturewith cooling
2. temperaturemaintaining the temperature below 20° C
3. customA precipitate formed overnight
4. temperaturethe orange suspension was heated
5. temperatureto reflux for 1 hour
6. temperatureThe suspension was cooled to room temperature
7. waitto stand overnight
8. stirringwithout stirring
9. filtrationThe suspension was filtered
10. additionthe filtrates were slowly diluted with water (200 mL)
11. customto give a yellow suspension
12. stirringThis suspension was stirred for two hours
13. customthe solids were collected
14. washwashed with water, aqueous methanol, 50% methanol/ether, and ether