反应详情

温度

60 °C

Add N-iodosuccinimide (14.19 g, 74.63 mmol) to ((R)-2-benzyloxy-1-hydroxymethylethyl)-carbamic acid tert-butyl ester (15.00 g, 53.30 mmol) and 2,2-dimethyl-1-vinyloxypropane (9.13 g, 79.96 mmol) in acetonitrile (267 mL) at room temperature. Heat to 60° C. under nitrogen for 2 hours. Cool to room temperature and dilute with ethyl acetate. Wash with water and saturated aqueous sodium chloride. Dry (magnesium sulfate), filter, concentrate and purify (silica gel chromatography, eluting with 0:100 to 10:90 ethyl acetate:hexanes) to give the desired compound as an oil (23.4 g 84.2%).

1. temperatureCool to room temperature
2. washWash with water and saturated aqueous sodium chloride
3. dry with materialDry (magnesium sulfate)
4. filtrationfilter
5. concentrationconcentrate
6. custompurify
7. wash(silica gel chromatography, eluting with 0:100 to 10:90 ethyl acetate:hexanes)