反应详情

温度

0 °C

At 0° C. TEA (44 μl, 0.314 mmol, 2 eq.) was added to (3-fluoro-pyridin-4-yl)-methanol (20 mg, 0.157 mmol, 1 eq.) in 1 mL DCM, followed by MsCl (15 μl, 0.188 mmol, 1.2 eq.) The reaction was stirred at 0° C. for 30 minutes. HPLC and LC-MS showed reaction complete. The reaction crude was concentrated down. Ethyl acetate was added and washed with saturated NAHCO3 aqueous solution. The Ethyl acetate layer was concentrated after dried over Na2SO4 to give color oil which was used directly in next step. LC-MS shows 206.1 (M+1).

1. customAt 0° C
2. customreaction complete
3. customThe reaction crude
4. concentrationwas concentrated down
5. additionEthyl acetate was added
6. washwashed with saturated NAHCO3 aqueous solution
7. concentrationThe Ethyl acetate layer was concentrated
8. dry with materialafter dried over Na2SO4
9. customto give color oil which