反应详情

温度

0 °C

2-(6-Bromopyridin-2-yl)-2-morpholin-4-ylethanol (Example 141, Step 1) (1 g, 3.48 mmol) was taken up in THF (7 mL) and cooled to 0° C. Sodium hydride (0.153 g, 3.83 mmol) was added and the suspension stirred at 0° C. for 5 minutes. A solution of iodomethane (0.240 mL, 3.83 mmol) in THF (3 mL) was added and the reaction mixture stirred at 0° C. for 30 minutes. Saturated NH4Cl was added and the reaction mixture was extracted with EtOAc (2×). The combined organic extracts were dried over MgSO4, filtered, and concentrated in vacuo. Purification of the residue by silica gel column chromatography (40-100% EtOAc-hexanes) gave the title compound as a yellow oil.

1. stirringthe reaction mixture stirred at 0° C. for 30 minutes
2. extractionthe reaction mixture was extracted with EtOAc (2×)
3. dry with materialThe combined organic extracts were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification of the residue by silica gel column chromatography (40-100% EtOAc-hexanes)