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温度

0 °C

HATU (105 mg, 0.28 mmol) and Cbz-N(Me)Ala-OH (65 mg, 0.28 mmol) were dissolved in NMP (0.5 mL) and DIPEA (65 μL, 0.36 mmol) was added. The reaction mixture was cooled to 0° C. and a solution of 30 (106 mg, 0.25 mmol) in NMP (2 mL) was added. The reaction mixture was warmed to ambient temperature. After 12 h, the reaction mixture was quenched with 1N NaOH (0.5 mL) and diluted with water, extracted with 10:1 Et2O/EtOAc. The combined organic extracts were washed successively with water, saturated aqueous NaHCO3, and brine, dried over anhydrous Na2SO4, filtered, and concentrated to afford 180 mg (100%) of 31 as a beige-colored foam which was used without further purification. Mass spectrum, m/z [651.2] (M+H)+.

1. temperatureThe reaction mixture was warmed to ambient temperature
2. customthe reaction mixture was quenched with 1N NaOH (0.5 mL)
3. additiondiluted with water
4. extractionextracted with 10:1 Et2O/EtOAc
5. washThe combined organic extracts were washed successively with water, saturated aqueous NaHCO3, and brine
6. dry with materialdried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated