反应详情

A mixture of 6-bromo-4-chloro-3-nitro-quinoline (Stage A.4, 1.1 g, 3.83 mmol) and 3,5-dimethyl-4-aminoisoxazol (Aldrich, Buchs, Switzerland, 472 mg, 4.21 mmol) in acetic acid (10 ml) was stirred at it for 4 h. Then the RM was quenched with H2O (40 ml). The suspension was filtered, the solid cake was washed with H2O (2×) and dried under vacuum, before being dissolved in EtOAc. The solution was washed with saturated aqueous NaHCO3, dried over Na2SO4, filtered and evaporated to dryness to give the title compound as an orange solid (HPLC tR 2.96 min (Method A); M+H=363, 365; M−H=361, 363 MS-ES).

1. customThen the RM was quenched with H2O (40 ml)
2. filtrationThe suspension was filtered
3. washthe solid cake was washed with H2O (2×)
4. customdried under vacuum
5. dissolutionbefore being dissolved in EtOAc
6. washThe solution was washed with saturated aqueous NaHCO3
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. customevaporated to dryness