反应详情

温度

50 °C

1-(5′-Hydroxy-2′-nitrophenyl)-2-propen-1-ol (2.0 g) is dissolved in dry dimethylformamide (100 ml) and thereto are added sodium iodide (1 equivalent) and potassium carbonate and 3-t-butoxycarbonylaminopropyl tosylate (1.5 equivalent). The mixture is stirred at 50° C. for 6 hours, and thereto is added ethyl acetate. The mixture is washed with an aqueous saturated saline solution, dried over sodium sulfate. After distilling off the solvent, the residue is purified with a silica gel column chromatography to give 1-[5′-(3″-t-butoxycarbonylaminopropyloxy)-2′-nitrophenyl]-2-propen-1-ol (3.53 g) as pale brown caramel.

1. washThe mixture is washed with an aqueous saturated saline solution
2. dry with materialdried over sodium sulfate
3. distillationAfter distilling off the solvent
4. customthe residue is purified with a silica gel column chromatography