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温度

0 °C

{4-[(4-Chloropyrimidin-2-yl)methyl]morpholin-3-yl}methanol (200 mg, 0.821 mmol) was taken up in DCM (4 mL) and cooled to 0° C. DAST (0.119 mL, 0.903 mmol) was added and the resulting mixture stirred at 0° C. for 90 minutes. Saturated NaHCO3 was added and the products extracted into EtOAc (2×). The combined organic extracts were washed with brine, dried over MgSO4, filtered, and concentrated in vacuo. Purification of the residue by silica gel chromatography (12-100% EtOAc-hexanes) followed by HPLC (10-40% MeCN—H2O) gave the title compound as a pale yellow gum.

1. extractionthe products extracted into EtOAc (2×)
2. washThe combined organic extracts were washed with brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification of the residue by silica gel chromatography (12-100% EtOAc-hexanes)