反应详情

To a solution of 4-benzyl-5-methyl-[1,4]oxazepane (0.30 g, 1.4 mmol) in 1,2-dichloroethane (3 mL) was added chloroethyl chloroformate (0.56 mL, 7 mmol) at room temperature. The mixture was refluxed for 10 hours and concentrated. The resulting residue was dissolved in methanol (5 mL) and the solution was refluxed for one hour. After concentration, the residual material was triturated, washed with ethyl acetate and collected by filtration to afford 5-methyl-[1,4]oxazepane hydrochloride (0.16 g, 1.1 mmol, 76%) as a white solid.

1. temperatureThe mixture was refluxed for 10 hours
2. concentrationconcentrated
3. dissolutionThe resulting residue was dissolved in methanol (5 mL)
4. temperaturethe solution was refluxed for one hour
5. concentrationAfter concentration
6. customthe residual material was triturated
7. washwashed with ethyl acetate
8. filtrationcollected by filtration