反应详情

温度

0 °C

Into a 250 mL 3-necked round bottom flask was placed a solution of benzyl 3-hydroxypyrrolidine-1-carboxylate (10 g, 45.23 mmol) in CH2Cl2 (100 mL). To this was added 3,4-dihydro-2H-pyran (19 g, 226.19 mmol). To the mixture was added p-toluenesulfonic acid (389 mg, 2.26 mmol) and the resulting solution was allowed to react, with stirring, for 10 minutes while the temperature was maintained at 0° C. The resulting solution was allowed to react, with stirring, for an additional 1 hour at room temperature. The reaction progress was monitored by TLC (ethyl acetate/petroleum ether=1:2). The reaction mixture was then quenched by the adding 100 mL of NaHCO3. The resulting mixture was washed with 100 mL of NaHCO3 and 100 mL of brine. The mixture was dried over MgSO4 and concentrated under vacuum using a rotary evaporator. This resulted in 15 g (98%) of benzyl 3-(tetrahydro-2H-pyran-2-yloxy)pyrrolidine-1-carboxylate as yellow oil.

1. customInto a 250 mL 3-necked round bottom flask was placed
2. customto react
3. customto react
4. stirringwith stirring, for an additional 1 hour at room temperature
5. customThe reaction mixture was then quenched by the adding 100 mL of NaHCO3
6. washThe resulting mixture was washed with 100 mL of NaHCO3 and 100 mL of brine
7. dry with materialThe mixture was dried over MgSO4
8. concentrationconcentrated under vacuum
9. customa rotary evaporator
10. customThis resulted in 15 g (98%) of benzyl 3-(tetrahydro-2H-pyran-2-yloxy)pyrrolidine-1-carboxylate as yellow oil