反应详情

温度

-20 °C

To a cooled (−20° C.) solution of 1-(4-fluorobenzyl)piperidine (17 g, 82 mmol) in anhydrous THF (200 mL) was added LiHMDS (1.0M in THF, 180 mL, 180 mmol) over a period of 15 min. The reaction mixture was stirred for 30 min at −20° C., then methyl phenylsulfinate (15 g, 98 mmol) was added over a period of 5 min. After being stirred at −20° C. for 1 hour, the reaction was quenched by the addition of water (100 mL). EtOAc (200 mL) was added and the organic layer was separated and washed with water (3×100 mL) and brine. The organic layer was dried over Mg2SO4, filtered, concentrated under vacuum. The crude product was used without purification in the next step.

1. stirringAfter being stirred at −20° C. for 1 hour
2. customthe reaction was quenched by the addition of water (100 mL)
3. additionEtOAc (200 mL) was added
4. customthe organic layer was separated
5. washwashed with water (3×100 mL) and brine
6. dry with materialThe organic layer was dried over Mg2SO4
7. filtrationfiltered
8. concentrationconcentrated under vacuum
9. customThe crude product was used without purification in the next step