反应详情

3-Nitrobenzyl bromide (10.0 g, 46 mmol) was dissolved in DMF (180 ml) and potassium carbonate (12.7 g, 92 mmol) added, followed by L-phenylalanine ethyl ester hydrochloride (10.6 g, 46 mmol). The reaction was stirred for 17 h at room temperature before evaporating to dryness. The residue was re-dissolved in EtOAc (150 ml) and washed with water (3×80 ml), dried (Na2SO4) filtered and concentrated to dryness. After purification by flash column chromatography (30% EtOAc/hexane) the product was obtained (3.7 g, 24% yield). LCMS purity 86%, m/z 329 [M++H]+.

1. custombefore evaporating to dryness
2. dissolutionThe residue was re-dissolved in EtOAc (150 ml)
3. washwashed with water (3×80 ml)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated to dryness
7. customAfter purification by flash column chromatography (30% EtOAc/hexane) the product
8. customwas obtained (3.7 g, 24% yield)