反应详情

To a solution of 2-benzyloxy-N,N′-bis(t-butoxycarbonyl)-N,N′-dimethyl-1,3-propanediamine (73.0 mg, 0.17 mmol) in methylene chloride (2.0 mL) was added a 4.0 M solution of hydrogen chloride in ethyl acetate (1.0 mL, 4.0 mmol), and the mixture was stirred at room temperature for 4 hours. The reaction mixture was concentrated under reduced pressure, ethanol (5.0 mL) was added to the residue, and the resulting mixture was concentrated under reduced pressure. An approx. 10% solution of ammonia in methanol (2.0 mL, approx. 12 mmol) was added to the residue, insoluble materials were removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel to yield the title compound as a colorless oil (35.0 mg, yield: 98%).

1. concentrationThe reaction mixture was concentrated under reduced pressure, ethanol (5.0 mL)
2. additionwas added to the residue
3. concentrationthe resulting mixture was concentrated under reduced pressure
4. customwere removed by filtration
5. concentrationthe filtrate was concentrated under reduced pressure
6. customThe residue was purified by column chromatography on silica gel