反应详情

To a solution of [5-(2-fluoro-6-trifluoromethyl-pyridin-4-yl)imidazo[1,2-a]pyrazin-8-yl]-(4-morpholin-4-yl-phenyl)carbamic acid tert-butyl ester (92 mg, 0.12 mmol) in THF (0.5 mL) is added KOtBu (26 mg, 0.23 mmol) and the mixture is stirred at rt for 20 min. HCl (12 M aq., 0.1 mL) is added and the mixture is diluted with water (10 mL) and concentrated under reduced pressure. The residue is dissolved in THF (5 mL) and HCl (12 M aq., 0.5 mL) is added and the mixture is stirred at rt for 5 h. NaHCO3 (sat. aq.) is added until the pH is 7 and the mixture is extracted with DCM (3×10 mL). The extracts are dried over Na2SO4 and evaporated under reduced pressure to afford a pale orange solid. This is purified by preparative HPLC to afford the title compound as a yellow solid (9.5 mg). LCMS: Rt=1.04 min (100%), m/z (ESI) 457 (M+H)+.

1. concentrationconcentrated under reduced pressure
2. dissolutionThe residue is dissolved in THF (5 mL)
3. additionHCl (12 M aq., 0.5 mL) is added
4. stirringthe mixture is stirred at rt for 5 h
5. additionNaHCO3 (sat. aq.) is added until the pH is 7
6. extractionthe mixture is extracted with DCM (3×10 mL)
7. dry with materialThe extracts are dried over Na2SO4
8. customevaporated under reduced pressure
9. customto afford a pale orange solid
10. customThis is purified by preparative HPLC