1-amino-3-(dibenzylamino)propan-2-ol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 2-chloroacetyl chloride (1.25 g, 10.96 mmol) in CHCl3 was added to the solution of 1-amino-3-(dibenzylamino)propan-2-ol (2.5 g, 9.26 mmol) in CHCl3 (50 mL) in ice-bath. The mixture was stirred for 1 hour, then stirred at room temperature for 2 hours. The organic layer concentrated, the residue was purified by column to give white solid. stirred at room temperature for 2 hours The organic layer concentrated the residue was purified by column to give white solid

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 2-(3-(dibenzylamino)-2-hydroxypropyl)isoindoline-1,3-dione (4.5 g, 11.25 mmol) in conc. HCl (50 mL) was stirred at 120° C. overnight. After cooling to room temperature, the mixture was filtered. And the filtrate was extracted with CHCl3. The aqueous layer was added aq. 30% NaOH until pH was above 7, then the solution was extracted with CH2Cl2, dried over Na2SO4 and concentrated to give yellow solid (3.0 g). the mixture was filtered And the filtrate was extracted with CHCl3 The aqueous layer was added aq. 30% NaOH until pH was above 7 the solution was extracted with CH2Cl2 dried over Na2SO4 concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 2-chloroacetyl chloride (1.25 g, 10.96 mmol) in CHCl3 was added to the solution of 1-amino-3-(dibenzylamino)propan-2-ol (2.5 g, 9.26 mmol) in CHCl3 (50 mL) in ice-bath. The mixture was stirred for 1 hour, then stirred at room temperature for 2 hours. The organic layer concentrated, the residue was purified by column to give white solid. stirred at room temperature for 2 hours The organic layer concentrated the residue was purified by column to give white solid

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 2-(3-(dibenzylamino)-2-hydroxypropyl)isoindoline-1,3-dione (4.5 g, 11.25 mmol) in conc. HCl (50 mL) was stirred at 120° C. overnight. After cooling to room temperature, the mixture was filtered. And the filtrate was extracted with CHCl3. The aqueous layer was added aq. 30% NaOH until pH was above 7, then the solution was extracted with CH2Cl2, dried over Na2SO4 and concentrated to give yellow solid (3.0 g). the mixture was filtered And the filtrate was extracted with CHCl3 The aqueous layer was added aq. 30% NaOH until pH was above 7 the solution was extracted with CH2Cl2 dried over Na2SO4 concentrated

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 2-chloroacetyl chloride (1.25 g, 10.96 mmol) in CHCl3 was added to the solution of 1-amino-3-(dibenzylamino)propan-2-ol (2.5 g, 9.26 mmol) in CHCl3 (50 mL) in ice-bath. The mixture was stirred for 1 hour, then stirred at room temperature for 2 hours. The organic layer concentrated, the residue was purified by column to give white solid. stirred at room temperature for 2 hours The organic layer concentrated the residue was purified by column to give white solid

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A solution of 2-(3-(dibenzylamino)-2-hydroxypropyl)isoindoline-1,3-dione (4.5 g, 11.25 mmol) in conc. HCl (50 mL) was stirred at 120° C. overnight. After cooling to room temperature, the mixture was filtered. And the filtrate was extracted with CHCl3. The aqueous layer was added aq. 30% NaOH until pH was above 7, then the solution was extracted with CH2Cl2, dried over Na2SO4 and concentrated to give yellow solid (3.0 g). the mixture was filtered And the filtrate was extracted with CHCl3 The aqueous layer was added aq. 30% NaOH until pH was above 7 the solution was extracted with CH2Cl2 dried over Na2SO4 concentrated