反应详情

To a solution of tert-butyl 3-bromo-5-(hydroxymethyl)benzoate (0.8 g, 2.79 mmol) in dichloromethane (14 mL) at 0° C. was added Dess-Martin reagent (1.54 g, 3.62 mmol). The mixture was warmed to ambient temperature. After 1 h, saturated NaHCO3 and saturated Na2SO3 were added the mixture was extracted with dichloromethane (3×) The combined organic extracts were washed with brine, dried over sodium sulfate, filtered and concentrated. Purification by silica gel chromatography (100% hexanes→80% hexanes/ethyl acetate) gave the title compound (440 mg).

1. extractionwas extracted with dichloromethane (3×) The combined organic extracts
2. washwere washed with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customPurification by silica gel chromatography (100% hexanes→80% hexanes/ethyl acetate)