反应详情

A mixture of 9-hydroxy-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (7.46 g, 41.6 mmol), benzyl bromide (Preparation 58) (5.45 ml, 45.8 mmol) and potassium carbonate (17.26 g, 125 mmol) was stirred and heated at 60° C. in DMF (75 ml) for 2 hours. Cooled, diluted with water (300 ml) and extracted with EtOAc (200 ml and 4×75 ml) and the combined organics washed with 3×100 ml of water. Dried (magnesium sulphate), evaporated, triturated with ether and filtered off to give 7.55 g of white solid. MS (ES): C16H15NO3 requires 269; found 270 [M+H]+.

1. temperatureCooled
2. extractionextracted with EtOAc (200 ml and 4×75 ml)
3. washthe combined organics washed with 3×100 ml of water
4. dry with materialDried (magnesium sulphate)
5. customevaporated
6. customtriturated with ether
7. filtrationfiltered off