反应详情

6.23 g (26.8 mmol) of benzylbis(2-chloroethyl)amine hydrochloride were dissolved in ethanol (100 ml) and, while stirring, 5.00 g (26.8 mmol) of N-Boc-3-aminopyrrolidine and 9.02 g (107 mmol) of sodium bicarbonate were added. The resulting reaction solution was heated under reflux for 4 h. The cooled reaction mixture was concentrated in vacuo, 100 ml of water were added, and the aqueous phase was extracted with ethyl acetate (4×60 ml). The combined organic phases were washed with saturated aqueous NaHCO3 solution, dried over magnesium sulfate and concentrated in vacuo. The residue was purified by chromatography on silica gel (mobile phase gradient 0-5% methanol in dichloromethane). Yield: 6.15 g (66%) of yellow solid

1. customThe resulting reaction solution
2. temperaturewas heated
3. temperatureunder reflux for 4 h
4. customThe cooled reaction mixture
5. concentrationwas concentrated in vacuo, 100 ml of water
6. additionwere added
7. extractionthe aqueous phase was extracted with ethyl acetate (4×60 ml)
8. washThe combined organic phases were washed with saturated aqueous NaHCO3 solution
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated in vacuo
11. customThe residue was purified by chromatography on silica gel (mobile phase gradient 0-5% methanol in dichloromethane)