反应详情

To a suspension of 3-{6-[2-(2-fluoro-4-trifluoromethyl-phenyl)-ethylamino]-2-methoxy-pyrimidin-4-yl}-phenol (280 mg, 0.68 mmol), and Cs2CO3 (0.44 g, 1.36 mmol) in DMF (2 mL) is added epichlorohydrin (80 μL, 1.02 mmol) at room temperature. After 4 h at 20° C., the mixture is diluted with water (10 mL), and extracted with EtOAc (2×10 mL). The extracts are washed with water (2×20 mL), dried (MgSO4), filtered, and concentrated. The residue is chromatographed on SiO2 eluting with 50%EtOAc in heptane to afford [2-(2-fluoro-4-trifluoromethyl-phenyl)-ethyl]-[2-methoxy-6-(3-oxiranylmethoxy-phenyl)-pyrimidin-4-yl]-amine [0.16 g, Example 66]. LCMS: RT=2.62 minutes; MS: 464 (M+H).

1. extractionextracted with EtOAc (2×10 mL)
2. washThe extracts are washed with water (2×20 mL)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue is chromatographed on SiO2 eluting with 50%EtOAc in heptane