反应详情

温度

60 °C

1M Lithium aluminum hydride (60 ml, 60.0 mmol) in THF was added to a stirred solution of 9-[(phenylmethyl)oxy]-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (Preparation 59) (7.4 g, 27.5 mmol) in THF (150 ml) under argon and heated at 60° C. for 2 hours then cooled and quenched by careful addition of 100 ml of 2M sodium hydroxide with ice bath cooling and the resulting suspension filtered, the solids washed with water and EtOAc and the organic dried (magnesium sulphate) and evaporated to give 7.01 g of white solid. MS (ES): C16H17NO2 requires 255; found 256 [M+H]+.

1. temperaturethen cooled
2. customquenched by careful addition of 100 ml of 2M sodium hydroxide with ice bath
3. temperaturecooling
4. filtrationthe resulting suspension filtered
5. washthe solids washed with water and EtOAc
6. dry with materialthe organic dried (magnesium sulphate)
7. customevaporated