反应详情

温度

0 °C

(4-Chloropyrimidin-2-yl)methanol (Example 548, Step 1) (121 mg, 0.84 mmol) was taken up in DCM (2.5 mL) and cooled to 0° C. DAST (0.122 mL, 0.92 mmol) was added and the resulting mixture stirred at 0° C. for 15 minutes and room temperature 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 (2-40% EtOAc-hexanes) gave the title compound as a pale yellow oil.

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 (2-40% EtOAc-hexanes)