反应详情

温度

0 °C

The Boc-containing compound 23 (1.0 g, 1.70 mmol) was dissolved in DCM (4 mL) and cooled to 0° C. before TFA (2 mL) was added and the reaction stirred at 0° C. for 1 h. TLC analysis (10:1 DCM/MeOH) indicated the starting material had all been consumed and the product had formed. The reaction mixture was concentrated at low pressure on the rotary evaporator. The crude residue was dissolved in DCM and washed successively with saturated aqueous NaHCO3 (3×), and brine. The organic layer was dried over anhydrous Na2SO4, filtered, and concentrated to afford 845 mg of 24 as a white foam. Mass spectrum, m/z [488.3] (M+H)+.

1. additionwas added
2. customall been consumed
3. customthe product had formed
4. concentrationThe reaction mixture was concentrated at low pressure on the rotary evaporator
5. dissolutionThe crude residue was dissolved in DCM
6. washwashed successively with saturated aqueous NaHCO3 (3×), and brine
7. dry with materialThe organic layer was dried over anhydrous Na2SO4
8. filtrationfiltered
9. concentrationconcentrated