反应详情

To a solution of 4-[3-(2-hydroxyethylamino)propyl]benzonitrile (4 g, 0.0196 mol; see step (v) above) in dry DCM (80 mL) were added, at 0-5° C., triethylamine (5.9 g, 0.0588 mol) and mesyl chloride (5.6 g, 0.049 mol). The resulting mixture was then stirred at room temperature for 30 min, after which the reaction was quenched by addition of water (50 mL). The resulting aqueous layer was extracted with DCM (2×50 mL) and the combined organic layers were washed with brine. Solvent was removed under reduced pressure and the crude product was recrystallised from methanol to yield 4.2 g (62%) of the title compound as a white solid.

1. customafter which the reaction was quenched by addition of water (50 mL)
2. extractionThe resulting aqueous layer was extracted with DCM (2×50 mL)
3. washthe combined organic layers were washed with brine
4. customSolvent was removed under reduced pressure
5. customthe crude product was recrystallised from methanol