反应详情

温度

25 °C

A mixture of 3-amino-5-hydroxyquinoxalin-2(1H)-one (0.067 g, 0.38 mmol, prepared as described in WO04014871), N-(2-(6-chloropyrimidin-4-yl)-5-(trifluoromethyl)-phenyl)-1-isobutylpiperidine-2-carboxamide, Example 39(e), (0.14 g, 0.32 mmol) and Cs2CO3 (0.12 g, 0.38 mmol, Strem) in DMF (2.5 mL) was stirred for 3 d at 25° C. The mixture was diluted with aqueous solution of NaHCO3 (100 mL) and extracted with 1:1 mixture of EtOAc/hexane (2×75 mL). The combined extracts were washed with H2O (2×75 mL) and brine (75 mL), dried over Na2SO4, filtered, and evaporated under reduced pressure. Purification of the residue by silica gel column chromatography (gradient: 25-60% EtOAc/hexane) afforded the title compound as a white solid. MS (ESI, pos. ion.) m/z: 582 (M+1). Mp: >250° C.

1. extractionextracted with 1:1 mixture of EtOAc/hexane (2×75 mL)
2. washThe combined extracts were washed with H2O (2×75 mL) and brine (75 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customevaporated under reduced pressure
6. customPurification of the residue by silica gel column chromatography (gradient: 25-60% EtOAc/hexane)