反应详情

To a solution of benzo[1,3]dioxole-4-carbaldehyde (10 g, 66.7 mmol) in 200 mL THF at −78° C. was added, via addition funnel, 43.7 mL of a 1.6 M MeLi solution in diethyl ether. The reaction was slowly warmed to room temperature and stirred overnight. A TLC of an aliquot showed reaction was complete. The reaction was then cooled to −78° C. and quenched with saturated aqueous ammonium chloride and concentrated in vacuo. The residue was then extracted with ethyl acetate. The organics were combined, dried over magnesium sulfate, and concentrated in vacuo to give 11 g (99.4% yield) of 1-benzo[1,3]dioxol-4-ylethanol as a brown oil that crystallized upon standing.

1. customreaction
2. temperatureThe reaction was then cooled to −78° C.
3. customquenched with saturated aqueous ammonium chloride
4. concentrationconcentrated in vacuo
5. extractionThe residue was then extracted with ethyl acetate
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated in vacuo