反应详情

To a solution Cbz-N(Me)-Ala-OH (1.2 g, 4.8 mmol) and HATU (2.0 g, 5.3 mmol) in NMP (30 mL) was added NMM (0.7 mL) followed by a solution of compound 33 (1.8 g, 4.0 mmol crude) in NMP (30 mL) at ambient temperature. After 16 h, the reaction mixture was diluted with 10% EtOAc in Et2O, washed successively with water, 1N HCl, 1N NaOH, and brine, dried over anhydrous Na2SO4, filtered, and concentrated. The crude residue was purified by RP-HPLC (2″ Dynamax® C18; 10-100% ACN/water containing 0.1% HOAc over 30 min; Flow: 40 mL/min) to afford 2.4 g of compound 34 as white solid. Mass spectrum, m/z [673.0] (M+H)+.

1. washwashed successively with water, 1N HCl, 1N NaOH, and brine
2. dry with materialdried over anhydrous Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customThe crude residue was purified by RP-HPLC (2″ Dynamax® C18
6. wait10-100% ACN/water containing 0.1% HOAc over 30 min