反应详情

A mixture of 1,2,3,4-tetrahydro-1-benzazepin-5-one (500 mg, 2.530 mmol), O-methyl hydroxylamine hydrochloride (211 mg, 2.530 mmol), sodium acetate (208 mg, 2.530 mmol) and sodium carbonate (536 mg, 5.060 mmol) in ethanol was refluxed for 3 hours. The resulting mixture was concentrated in vacuo to remove ethanol and to the residue was added water (15 mL). The residue in water was extracted with dichloromethane (15 mL×3). The organic layers were combined, dried over sodium sulfate, and concentrated in vacuo to afford 326 mg of the desired product (yield was 67%).

1. temperaturewas refluxed for 3 hours
2. concentrationThe resulting mixture was concentrated in vacuo
3. customto remove ethanol
4. additionto the residue was added water (15 mL)
5. extractionThe residue in water was extracted with dichloromethane (15 mL×3)
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated in vacuo