反应详情

A solution of 22 (222 mg, 0.3 mmol) in DCM (10 mL) was treated with TFA (3 mL) at ambient temperature. After 1.5 h, the solution was concentrated, diluted with EtOAc, washed with saturated NaHCO3, dried over anhydrous Na2SO4, filtered and concentrated. The resulting residue was diluted with ACN/H2O containing 0.1% HOAc and purified by reverse-phase HPLC (2″ Dynamax® C18, 10-100% ACN/H2O containing 0.1% HOAc). The product-containing fractions were frozen and lyophilized to afford 23 as a white solid.

1. concentrationthe solution was concentrated
2. additiondiluted with EtOAc
3. washwashed with saturated NaHCO3
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. additionThe resulting residue was diluted with ACN/H2O containing 0.1% HOAc
8. custompurified by reverse-phase HPLC (2″ Dynamax® C18, 10-100% ACN/H2O containing 0.1% HOAc)
9. temperatureThe product-containing fractions were frozen