反应详情

A solution of the crude phthalimide and hydrazine hydrate (10.0 ml, 177 mmol) in EtOH (200 ml) was stirred at reflux for 1 hour. Once cooled, the mixture was concentrated under reduced pressure. The residue was suspended in 1.5M HCl (200 ml) and washed with CH2Cl2 (50 ml×3). The organic solution was extracted with 4M HCl (50 ml×2). The combined aqueous extracts were made basic with 10M NaOH (100 ml) and extracted with CH2Cl2 (50 ml×4). This organic solution was dried (Na2SO4), filtered and concentrated under reduced pressure. Purification gave ((R)-2-amino-1-phenyl-ethyl)-carbamic acid tert-butyl ester as an off-white solid (2.41 g, 51% over 2 steps).

1. temperatureat reflux for 1 hour
2. temperatureOnce cooled
3. concentrationthe mixture was concentrated under reduced pressure
4. washwashed with CH2Cl2 (50 ml×3)
5. extractionThe organic solution was extracted with 4M HCl (50 ml×2)
6. extractionextracted with CH2Cl2 (50 ml×4)
7. dry with materialThis organic solution was dried (Na2SO4)
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customPurification