반응 #51961

반응 방정식

tert-butyl 2-{4-[(dimethylamino)methyl]phenyl}-2-hydroxyethyl(methyl)carbamate

→

title compound

수율 106.8%

1-{4-[(Dimethylamino)methyl]phenyl}-2-(methylamino)ethanol

수율 106.8%

용매

HCl dioxane

반응 조건

후처리

1. 1
   기타The solvent and HCl was evaporated
2. 2
   workup.ADDITIONAfter treated with high vacuum for 15 minutes
3. 3
   workup.DISSOLUTIONthe residue was dissolved in methanol (2 mL)
4. 4
   workup.ADDITIONtreated with resin (BioRad 50w×2, 0.20 g) for 3 hours
5. 5
   여과The resin was collected by filtration
6. 6
   세척washed with methanol
7. 7
   세척The product on the resin was washed off with NH4OH/CH3OH (20 mL, 10% ammonium hydroxide aqueous solution (Aldrich, 29.4% NH3) in methanol)
8. 8
   농축The solution was concentrated to dryness
9. 9
   workup.ADDITIONtreated with high vacuum

실험 절차

To a solution of HCl-dioxane (20 mL, 4.0 M HCl in dioxane) was added tert-butyl 2-{4-[(dimethylamino)methyl]phenyl}-2-hydroxyethyl(methyl)carbamate (124 mg, 0.40 mmol). The mixture was stirred at room temperature for 16 hours. The solvent and HCl was evaporated. After treated with high vacuum for 15 minutes, the residue was dissolved in methanol (2 mL) and treated with resin (BioRad 50w×2, 0.20 g) for 3 hours. The resin was collected by filtration and washed with methanol. The product on the resin was washed off with NH4OH/CH3OH (20 mL, 10% ammonium hydroxide aqueous solution (Aldrich, 29.4% NH3) in methanol). The solution was concentrated to dryness, and treated with high vacuum to give the title compound (89 mg) as an oil.

출처