反应详情

To a stirred solution of methyl (tert-butyloxycarbonyl)glycinate (8.54 g, 45.1 mmol) was added hydrazine hydrate (4.4 mL, 90.5 mmol) and the reaction was heated under reflux for 16 hours. The solvent was removed in vacuo and the residue partitioned between dichloromethane (100 mL) and water (100 mL). The phases were separated, the aqueous phase evaporated in vacuo to low volume and extracted with 5% methanol/dichloromethane (2×100 mL) The organic extracts were combined, dried over magnesium sulfate and concentrated in vacuo to give the product as a white crystalline solid, 5.27 g (62%).

1. temperaturethe reaction was heated
2. temperatureunder reflux for 16 hours
3. customThe solvent was removed in vacuo
4. customthe residue partitioned between dichloromethane (100 mL) and water (100 mL)
5. customThe phases were separated
6. customthe aqueous phase evaporated in vacuo to low volume
7. extractionextracted with 5% methanol/dichloromethane (2×100 mL) The organic extracts
8. dry with materialdried over magnesium sulfate
9. concentrationconcentrated in vacuo