反应详情

A solution of hydroxylamine hydrochloride (2.38 g, 34.2 mmole) in 1:1 ethanol/pyridine (100 mL) was added to a solution of 1-[(3S)-5-hydroxy-3-(hydroxymethyl)-2,3-dihydro-1,4-benzodioxin-6-yl]-1-ethanone (1.92 g, 8.57 mmole) in ethanol (200 mL). It was then heated to reflux under nitrogen for 5 hours. Upon cooling, the solvent was removed and replaced with ethyl acetate. The solution was then washed with water (200 mL) and with aqueous 2N HCl (100 mL), dried over magnesium sulfate, filtered and evaporated in vacuum to give 1.89 g (93%) of the (S)-enantiomer of the title compound as a gray solid, m.p. 162° C. MS (ESI) m/z 240 (M+H)+.

1. temperatureIt was then heated
2. temperatureto reflux under nitrogen for 5 hours
3. temperatureUpon cooling
4. customthe solvent was removed
5. washThe solution was then washed with water (200 mL) and with aqueous 2N HCl (100 mL)
6. dry with materialdried over magnesium sulfate
7. filtrationfiltered
8. customevaporated in vacuum