反应详情

To a solution of 1,3-propanediamine (6.50 g, 87.0 mol) in 250 mL of abs. EtOH was added benzyl phenyl carbonate (20.0 g, 87.0 mmol). The solution was stirred overnight. A white precipitate formed. The solvent was removed in a rotary evaporator, and the residue was taken up with 100 ml of distilled H2O. This was followed by acidification with 2M HCl to pH 1-2, and 4× extracting with 250 mL of CH2Cl2 each time. The aqueous phase was rendered strongly alkaline with 2M NaOH and extracted 4× with 250 mL of CH2Cl2 each time. The combined organic phases were dried over Na2SO4, subsequently the solvent was removed in a rotary evaporator to obtain the product as a viscid white mass (4.70 g, 26%).

1. customA white precipitate formed
2. customThe solvent was removed in a rotary evaporator
3. extractionextracting with 250 mL of CH2Cl2 each time
4. extractionextracted 4× with 250 mL of CH2Cl2 each time
5. dry with materialThe combined organic phases were dried over Na2SO4
6. customsubsequently the solvent was removed in a rotary evaporator
7. customto obtain the product as a viscid white mass (4.70 g, 26%)