反应详情

A solution of benzyl 3-[(1E)-N-(tert-butoxycarbonyl)-4,4-dimethoxybutanehydrazonoyl]azetidine-1-carboxylate (2.47 g, 5.67 mmol) and AcOH (30 mL) was stirred (40° C.) for 18 h. The mixture was concentrated and the residue was dissolved in EtOAc (75 mL) and washed with saturated, aqueous NaHCO3 (75 mL). The aqueous layer was extracted with EtOAc (2×50 mL) and the combined organic layers were washed with brine, dried (Na2SO4) and concentrated to afford the desired product (2.1 g) which was used without further purification. ES-MS m/z 272.01 [M+H]+, HPLC RT (min) 3.50.

1. concentrationThe mixture was concentrated
2. dissolutionthe residue was dissolved in EtOAc (75 mL)
3. washwashed with saturated, aqueous NaHCO3 (75 mL)
4. extractionThe aqueous layer was extracted with EtOAc (2×50 mL)
5. washthe combined organic layers were washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated