庚基 甲磺酸盐

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of [(R)-1-hydroxymethyl-3-(4-hydroxy-phenyl)-1-methyl-propyl]-carbamic acid tert-butyl ester (2.06 g, 6.98 mMol) in ethanol (100 ml) is added potassium carbonate (2.90 g, 20.8 mMol) and methanesulfonic acid heptyl ester (2.04 g, 10.5 mMol). The mixture is heated to reflux temperature and stirred at that temperature for 6 hours. The mixture is then cooled to RT and stirred at RT overnight. The reaction mixture is then poured onto a biphasic mixture of AcOEt and HCl (aqueous, 1 M). The aqueous phase is extracted twice with AcOEt. The combined organic layers are washed with NaHCO3 (saturated aqueous solution), dried (Na2SO4) and concentrated under reduced pressure. Column chromatography eluting with 8% AcOEt in toluene gives the title compound as a colourless oil. The mixture is heated to reflux temperature stirred at RT overnight The aqueous phase is extracted twice with AcOEt The combined organic layers are washed with NaHCO3 (saturated aqueous solution) dried (Na2SO4) concentrated under reduced pressure Column chromatography eluting with 8% AcOEt in toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of [(R)-1-hydroxymethyl-3-(4-hydroxy-phenyl)-1-methyl-propyl]-carbamic acid tert-butyl ester (2.06 g, 6.98 mMol) in ethanol (100 ml) is added potassium carbonate (2.90 g, 20.8 mMol) and methanesulfonic acid heptyl ester (2.04 g, 10.5 mMol). The mixture is heated to reflux temperature and stirred at that temperature for 6 hours. The mixture is then cooled to RT and stirred at RT overnight. The reaction mixture is then poured onto a biphasic mixture of AcOEt and HCl (aqueous, 1 M). The aqueous phase is extracted twice with AcOEt. The combined organic layers are washed with NaHCO3 (saturated aqueous solution), dried (Na2SO4) and concentrated under reduced pressure. Column chromatography eluting with 8% AcOEt in toluene gives the title compound as a colourless oil. The mixture is heated to reflux temperature stirred at RT overnight The aqueous phase is extracted twice with AcOEt The combined organic layers are washed with NaHCO3 (saturated aqueous solution) dried (Na2SO4) concentrated under reduced pressure Column chromatography eluting with 8% AcOEt in toluene

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a stirred solution of [(R)-1-hydroxymethyl-3-(4-hydroxy-phenyl)-1-methyl-propyl]-carbamic acid tert-butyl ester (2.06 g, 6.98 mMol) in ethanol (100 ml) is added potassium carbonate (2.90 g, 20.8 mMol) and methanesulfonic acid heptyl ester (2.04 g, 10.5 mMol). The mixture is heated to reflux temperature and stirred at that temperature for 6 hours. The mixture is then cooled to RT and stirred at RT overnight. The reaction mixture is then poured onto a biphasic mixture of AcOEt and HCl (aqueous, 1 M). The aqueous phase is extracted twice with AcOEt. The combined organic layers are washed with NaHCO3 (saturated aqueous solution), dried (Na2SO4) and concentrated under reduced pressure. Column chromatography eluting with 8% AcOEt in toluene gives the title compound as a colourless oil. The mixture is heated to reflux temperature stirred at RT overnight The aqueous phase is extracted twice with AcOEt The combined organic layers are washed with NaHCO3 (saturated aqueous solution) dried (Na2SO4) concentrated under reduced pressure Column chromatography eluting with 8% AcOEt in toluene