反应详情

温度

0 °C

To a solution of 3-(2-chloro-5-nitro-phenoxymethyl)-azetidine-1-carboxylic acid tert-butyl ester (2.5 g, 7.29 mmol) in 60 mL of MeOH/H2O (1:1) and 3 mL of acetic acid (J. T. Baker) was added Zn powder (2.3 g, 36.47 mmol, Aldrich) at 0° C. The reaction mixture was stirred at 0° C. for 2 h then stirred at 10° C. for 2 h. The resulting mixture was filtered through a Celite® pad and the filtrate was concentrated in vacuo. The residue was treated with 60 mL of saturated aqueous NaHCO3 and extracted with EtOAc (3×50 mL). The combined organic layers were washed with brine and dried with MgSO4. The resulting solution was concentrated in vacuo and the title compound was obtained by column chromatography (silica gel, EtOAc) as a yellow solid.

1. stirringthen stirred at 10° C. for 2 h
2. filtrationThe resulting mixture was filtered through a Celite® pad
3. concentrationthe filtrate was concentrated in vacuo
4. additionThe residue was treated with 60 mL of saturated aqueous NaHCO3
5. extractionextracted with EtOAc (3×50 mL)
6. washThe combined organic layers were washed with brine
7. dry with materialdried with MgSO4
8. concentrationThe resulting solution was concentrated in vacuo