反应详情

温度

-20 °C

44 g BocGlyOH (0.25 moles) is dissolved in 250 ml DMF, together with 29 g HOSu. After cooling to -20° C. 52 g DCC dissolved in 250 ml DMF is added. After 4 hours stirring at room temperature 95 g ValOBzl, pTos is added together with 35 ml TEA. After stirring overnight at room temperature, DCU is filtered off, DMF removed and the resulting oil taken up in EtAc and washed with sat. NaCl, sat. NaHCO, and 10% citric acid. The EtAc is dried with Na2SO4, removed by vacuum evaporation and the resulting crystalline mass dried in a desiccator. Yield: 59 g (65%).

1. additionis added
2. filtrationDCU is filtered off
3. customDMF removed
4. washwashed with sat. NaCl, sat. NaHCO, and 10% citric acid
5. dry with materialThe EtAc is dried with Na2SO4
6. customremoved by vacuum evaporation
7. customthe resulting crystalline mass dried in a desiccator