反应详情

温度

105 °C

9-(Methyloxy)-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (Preparation 57) (9.3 g, 48.1 mmol) in hydrobromic acid (120 ml, 2210 mmol) was stirred and heated at 105° C. for 5 hours. Evaporated to dryness, azeotroped with 200 ml of ethanol and biotage chromatographed twice in 3% methanol in EtOAc. Triturated with EtOAc and filtered off to give 6.61 g of white solid. MS (ES): C9H9NO3 requires 179; found 180 [M+H]+.

1. customEvaporated to dryness
2. customazeotroped with 200 ml of ethanol and biotage
3. customchromatographed twice in 3% methanol in EtOAc
4. customTriturated with EtOAc
5. filtrationfiltered off