反应详情

A solution of benzylchloroformate (10.48 ml, 74 mmol) in dichloromethane (250 ml) was added to an ice-cooled solution of 4-aminomethyl benzylamine (10 g, 74 mmol) and triethylamine (9.77 ml, 74 mmol), in dichloromethane (480 ml) over 90 minutes. The mixture was concentrated under reduced pressure and the residue partitioned between ethyl acetate (450 ml) and 1M sodium hydroxide solution (300 ml). The resulting mixture was filtered, the layers separated and the organic phase dried over magnesium sulphate and evaporated under reduced pressure. The residue was dissolved in hot ethyl acetate, the solution cooled in an ice-bath, the resulting solid filtered off, and the filtrate evaporated under reduced pressure to afford the title compound as a white solid, 7.44 g.

1. concentrationThe mixture was concentrated under reduced pressure
2. customthe residue partitioned between ethyl acetate (450 ml) and 1M sodium hydroxide solution (300 ml)
3. filtrationThe resulting mixture was filtered
4. customthe layers separated
5. dry with materialthe organic phase dried over magnesium sulphate
6. customevaporated under reduced pressure
7. dissolutionThe residue was dissolved in hot ethyl acetate
8. temperaturethe solution cooled in an ice-bath
9. filtrationthe resulting solid filtered off
10. customthe filtrate evaporated under reduced pressure