反应详情

5-(3-Phthalimido-propyloxy)-1,3-bis-(hydroxymethyl)-benzene (1.45 g) was dissolved in a mixture of dichloromethane and ethanol (25 mL, 25:75). Hydrazine hydrate (0.62 mL) was added and the reaction mixture was refluxed for 1 h. The solvent was removed in vacuo and the residue dissolved in dichloromethane. The insoluble residue was filtered off and purified by silica gel chromatography (Merck SuperVarioPrep 70 g column, Si60 15-40 μm), eluted with methanol/dichloromethane, 20:80 then ammonium hydroxide/methanol/dichloromethane, 0.5:25:75 to give 1-(3-amino-propyloxy)-3,5-bis-(hydroxy-methyl)-benzene (1 g) suitable for further transformation.

1. temperaturethe reaction mixture was refluxed for 1 h
2. customThe solvent was removed in vacuo
3. dissolutionthe residue dissolved in dichloromethane
4. filtrationThe insoluble residue was filtered off
5. custompurified by silica gel chromatography (Merck SuperVarioPrep 70 g column, Si60 15-40 μm)
6. washeluted with methanol/dichloromethane, 20:80