反应详情

A mixture of (S)-4,6-dichloro-N-(1-methoxypropan-2-yl)pyrimidin-2-amine (260 mg, 0.11 mmol, Example 122(a)), hydriodic acid (57 wt. % in water, 40.4 μl, 0.165 mmol, Aldrich), sodium iodide (248 mg, 0.165 mmol) and DCM (5 mL) was stirred at room temperature for 2 h. The reaction mixture was diluted with EtOAc (50 mL), washed with 1N NaOH (2×25 mL) and brine (60 mL), dried over Na2SO4 and filtered. The filtrate was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (7% EtOAc/hexane) to give the title compound. MS (ESI, pos. ion) m/z: 420 (M+1).

1. washwashed with 1N NaOH (2×25 mL) and brine (60 mL)
2. dry with materialdried over Na2SO4
3. filtrationfiltered
4. customThe filtrate was evaporated under reduced pressure
5. customthe residue was purified by silica gel column chromatography (7% EtOAc/hexane)