反应详情

A solution of phenol-ether 78 (0.86 g, 1.8 mmol) in DCM (10 mL) was treated with TFA (3 mL) at 0° C. After 20 min, the reaction was warmed to ambient temperature. After 1 h, the solution was concentrated, diluted with EtOAc, washed successively with saturated aqueous NaHCO3, and brine, dried over anhydrous Na2SO4, filtered and concentrated. The aqueous phase was back-extracted with DCM and the combined organic extracts were concentrated to give amine 80 as an orange-colored oil that was used without further purification. Mass spectrum, m/z [389.5] (M+H)+.

1. waitAfter 1 h
2. concentrationthe solution was concentrated
3. additiondiluted with EtOAc
4. washwashed successively with saturated aqueous NaHCO3, and brine
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. extractionThe aqueous phase was back-extracted with DCM
9. concentrationthe combined organic extracts were concentrated