反应详情

温度

0 °C

To a stirring solution of 1-[3-(tert-butyldimethylsilyloxymethyl)-phenyl]-propan-2-ol (130 mg, 0.46 mmol) in THF (1.5 mL) under nitrogen at 0° C. was added diisopropyl azodicarboxylate (140 mg, 0.7 mmol), triphenylphosphine (180 mg, 0.7 mmol), and diphenylphosphoryl azide (190 mg, 0.7 mmol) and the mixture was stirred at 0° C. for 15 min. The mixture was diluted with dichloromethane, washed with water, brine, dried over magnesium sulfate, and purified by flash column chromatography (ethyl acetate/hexanes). 1H NMR (CDCl3) 7.27 (m, 1H), 7.2 (m, 1H), 7.16 (s, 1H), 7.08 (m, 1H), 4.74 (s, 2H), 3.65 (m, 1H), 2.82 (dd, 1H), 2.73 (dd, 1H), 1.25 (d, 3H), 0.94 (s, 9H), 0.10 (s, 6H).

1. washwashed with water, brine
2. dry with materialdried over magnesium sulfate
3. custompurified by flash column chromatography (ethyl acetate/hexanes)