反应详情

To a solution of 6.28 g (24.4 mmol) of 1-(1,1-dimethylethyl) 3-ethyl (3S)-piperidine-1,3-dicarboxylate in 25 mL of MeOH was added 7.11 mL of hydrazine monohydrate (146 mmol, 5.98 eq.). The mixture was refluxed for 2 h and concentrated. The reaction could be monitored by LC/MS on a reversed-phase column at 220 nm wavelength. The crude material was taken up in EtOAc, and washed with 2×H2O, 1× sat. aqueous NaCl, and dried over Na2SO4. Filtration and concentration afforded 3.21 g of product (54.0% yield) as a viscous oil. The product was ca. 80% pure by hplc analysis and was used as such without further purification.

1. temperatureThe mixture was refluxed for 2 h
2. concentrationconcentrated
3. customThe reaction
4. washwashed with 2×H2O, 1× sat. aqueous NaCl
5. dry with materialdried over Na2SO4
6. filtrationFiltration and concentration