反应详情

3-t-Butoxycarbonylaminopropanol (10.0 g) is dissolved in methylene chloride (100 ml) and thereto are added triethylamine (8.66 g) and tosyl chloride (16.3 g) with stirring under ice cooling. The mixture is stirred at room temperature overnight. The reaction mixture is concentrated and the residue is dissolved in water-ethyl acetate, and the organic layer is separated, washed with an aqueous saturated saline solution, dried over sodium sulfate, and then distilled off the solvent. The residue is purified with a silica gel column chromatography to give 3-t-butoxycarbonylaminopropyl tosylate (15.37 g) as pale yellow oil.

1. stirringThe mixture is stirred at room temperature overnight
2. concentrationThe reaction mixture is concentrated
3. dissolutionthe residue is dissolved in water-ethyl acetate
4. customthe organic layer is separated
5. washwashed with an aqueous saturated saline solution
6. dry with materialdried over sodium sulfate
7. distillationdistilled off the solvent
8. customThe residue is purified with a silica gel column chromatography