反应详情

To a stirred solution of 2-chloro-4-fluoro-3-(tetrahydro-pyran-2-yloxymethyl)-pyridine (0.20 g. 0.81 mmol) which was prepared according to the synthesis of 3-bromo-5-chloro-4-(tetrahydro-pyran-2-yloxymethyl)-pyridine in anhydrous MeOH (4 mL) was added Cs2CO3 (0.54 g. 1.6 mmol). After vigorous stirring for 20 h at room temperature acedic acid (92 μL. 1.6 mmol) was added the solvent was removed in vacuo and the residue was partitioned between DCM (20 mL) and water (4 mL). The organic layer was dried over Na2SO4 filtered and concentrated in vacuo. The resulting title compound was used for the next reaction without purification. MS (m/z): 257.9 [M+H+].

1. additionwas added the solvent
2. customwas removed in vacuo
3. customthe residue was partitioned between DCM (20 mL) and water (4 mL)
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe resulting title compound was used for the next reaction without purification