反应详情

To a mixture of dimethyl 5-bromo-7-ethyl-4-hydroxyquinoline -2,3-dicarboxylate (1.0 g, 2.7 mM,) in ethanol (25 mL) was added hydrazine hydrate (0.68 g, 14 mM). The resulting mixture was concentrated at 30° C. using a rotary evaporator and the residue was diluted with another portion of ethanol (25 mL) and similarly concentrated at 30° C. The residue was suspended in ethanol and filtered to separate the title compound (0.82 g, 82%) as a light yellow solid. Recrystallization of a portion of this material from dimethylsulfoxide/ethanol provided an analytical sample of the title compound as a light yellow crystalline solid, mp 335°-340° C. (dec). Analysis for C13H14BrN5O3 ·0.35 H2O Calculated: C, 41.70; H, 3.95; N, 18.70 Found: C, 41.99; H, 3.84; N, 18.31

1. concentrationThe resulting mixture was concentrated at 30° C.
2. customa rotary evaporator
3. additionthe residue was diluted with another portion of ethanol (25 mL)
4. concentrationsimilarly concentrated at 30° C
5. filtrationfiltered
6. customto separate the title compound (0.82 g, 82%) as a light yellow solid
7. customRecrystallization of a portion of this material from dimethylsulfoxide/ethanol