반응 #1702092
ord-b1d439d00c2d435ab18937b37453f277
반응 방정식
반응 조건
후처리
- 1기타The reaction was quenched by the addition of saturated NaHCO3
- 2기타The mixture was then partitioned between CH2Cl2 and H2O
- 3기타The layers were separated
- 4세척the organic layer was washed with brine
- 5건조dried over Na2SO4
- 6기타The drying agent was removed by vacuum filtration
실험 절차
The HCl salt of (2-amino-ethyl)-phosphonic acid diethyl ester (4.5 g, 20.7 mmol) was dissolved in CH2Cl2 (100 mL). To this solution was added CBzCl (3.2 mL, 22.7 mmol), followed by iPr2NEt (14.4 mL, 82.8 mmol). The reaction was stirred at room temperature until complete, as determined by TLC (eluent: 100% EtOAc). The reaction was quenched by the addition of saturated NaHCO3. The mixture was then partitioned between CH2Cl2 and H2O. The layers were separated and the organic layer was washed with brine and then dried over Na2SO4. The drying agent was removed by vacuum filtration and (2-benzyloxycarbonylamino-ethyl)-phosphonic acid diethyl ester was isolated from the concentrated filtrate by silica gel column chromatography (EtOAc/hexanes) (5.98 g, 92%).