反应详情

A solution of carbamate 90 (175 mg, 0.29 mmol) in DCM (10 mL) was treated with TFA (4 mL) at 0° C. After 1.5 h, the reaction mixture was concentrated, diluted with EtOAc, washed successively with saturated aqueous NaHCO3, and brine dried over anhydrous Na2SO4, filtered and concentrated. The crude residue was purified by reverse phase HPLC (2″ Dynamax® C18; 10% ACN/water to 70% ACN/water containing 0.1% HOAc, 30 min; Flow: 40 mL/min). The product-containing fractions were combined, frozen, and lyophilized to afford 91 (80 mg, 55%) as a white flocculent solid.

1. concentrationthe reaction mixture was concentrated
2. additiondiluted with EtOAc
3. washwashed successively with saturated aqueous NaHCO3, and brine
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude residue was purified by reverse phase HPLC (2″ Dynamax® C18
8. customto 70% ACN/water containing 0.1% HOAc, 30 min
9. temperaturefrozen