反应详情

To a solution of 4-(7-fluoro-2,3-dihydrobenzofuran-2-yl)piperidin-4-ol hydrochloride (380 mg, 1.388 mmol) in MeOH (11.1 mL) at 0° C. was added NBS (235 mg, 1.319 mmol) in one portion. Upon completion of addition, the reaction mixture was stirred at room temperature for 3 hours, and then quenched with aqueous Na2H2S2O5 (10%, 5 mL). The solvent was removed under reduced pressure to yield a residue. The residue was diluted with CH2Cl2 (5 mL), washed with aqueous NaOH (1 N, 3 mL) and brine (3 mL). The organic layer was separated, dried (K2CO3), filtered, and concentrated to afford Compound 1G as a white solid (0.168 g, 38% yield). LC/MS (m/z)=317 (M+H)+.

1. additionUpon completion of addition
2. customquenched with aqueous Na2H2S2O5 (10%, 5 mL)
3. customThe solvent was removed under reduced pressure
4. customto yield a residue
5. washwashed with aqueous NaOH (1 N, 3 mL) and brine (3 mL)
6. customThe organic layer was separated
7. dry with materialdried (K2CO3)
8. filtrationfiltered
9. concentrationconcentrated