反应详情

To a stirred suspension of 7-chloro-4-hydroxy-2-(4-methoxy-2-methylphenyl)-1,2,5,10-tetrahydropyridazino[4,5-b]quinoline-1,10-dione (400 mg, 1.03 mM) in methanol (4 mL) was added choline hydroxide (45% by weight in methanol, 295.6 uL, 1.03 mM). After brief sonication, all solids dissolved and the resulting solution was filtered through a Gelman Glass Acrodisc filter (0.45 um) along with an additional quantity of methanol (8 mL). The filtrate was concentrated to dryness and the residual oil was stirred with isopropanol (15 mL) and ethanol (8 mL) whereupon crystallization occurred. The solids were collected and dried under vacuum at 100° C. overnight to give the title compound (411 mg, 81%) as a yellow solid, mp 229°-230°C.

1. customAfter brief sonication
2. dissolutionall solids dissolved
3. filtrationthe resulting solution was filtered through a Gelman Glass Acrodisc
4. filtrationfilter (0.45 um) along with an additional quantity of methanol (8 mL)
5. concentrationThe filtrate was concentrated to dryness
6. customThe solids were collected
7. customdried under vacuum at 100° C. overnight