反应详情

温度

0 °C

At 0° C., to a 50 mL round bottomed flask charged with 1,1-dimethylethyl 3-pyrazolidinecarboxylate (0.054 g, 0.259 mmol) and stirrer in dichloromethane (DCM) (3 mL), was added triethylamine (0.079 mL, 0.569 mmol). After a couple of minutes, N-(benzyloxycarbonyloxy)succinimide (CBz-OSu) (0.064 g, 0.259 mmol) in dichloromethane (DCM) (1.5 mL) was added dropwise. The reaction mixture stirred at 0° C. for one hour, then warmed to r.t. After 2 hr at r.t., the solvent was evaporated and the residue was dissolved in EtOAc (30 mL), washed with water (15 mL×2), sat. NaHCO3 (15 ml), brine (15 mL), dried over Na2SO4 and concentrated to afford the crude product as a colorless gum (88 mg).

1. waitAfter a couple of minutes
2. temperaturewarmed to r.t
3. waitAfter 2 hr at r.t.
4. customthe solvent was evaporated
5. dissolutionthe residue was dissolved in EtOAc (30 mL)
6. washwashed with water (15 mL×2), sat. NaHCO3 (15 ml), brine (15 mL)
7. dry with materialdried over Na2SO4
8. concentrationconcentrated