反应详情

To a solution of 1,4-oxazepan-5-one (6.9 g, 60.0 mmol) in dichloromethane (120.0 mL) were added di-tert-butylcarbonate (1.75 g, 8.00 mmol) and dimethylaminopyridine (7.90 g, 65.0 mmol), and triethylamine (12.5 mL, 90.0 mmol) was added dropwise. After stirring for 16 hours at room temperature, to the mixture was added water, and the aqueous layer was extracted with chloroform. The organic layer was washed with saturated aqueous solution of ammonium chloride and brine, and then dried over sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified with silica gel column (hexane/ethyl acetate=90/10 to 0/100) to give the title compound (7.30 g, 37.2 mmol, 62%).

1. additionwas added dropwise
2. extractionthe aqueous layer was extracted with chloroform
3. washThe organic layer was washed with saturated aqueous solution of ammonium chloride and brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe obtained residue was purified with silica gel column (hexane/ethyl acetate=90/10 to 0/100)