反应详情

To a solution of 150 mg (R)-tert-butoxycarbonylamino-3-fluoropropionic acid in 2 ml DMF were added 115 mg 1-ethoxycarbonylpiperazine, 0.18 ml N-ethylmorpholine and 238 mg TOTU. After stirring for 12 h it was diluted with ethyl acetate and extracted with aqueous LiCl (4% w/w), aqueous NaHCO3, 0.1 M HCl and brine. The organic layer was dried over MgSO4 and concentrated to furnish the crude coupling product which was deprotected by using 10 equivalents TFA in dichloromethane. After stirring for 12 h it was concentrated and codistilled twice with toluene. Yield: 216 mg colorless oil.

1. extractionextracted with aqueous LiCl (4% w/w), aqueous NaHCO3, 0.1 M HCl and brine
2. dry with materialThe organic layer was dried over MgSO4
3. concentrationconcentrated
4. customto furnish the crude coupling product which
5. stirringAfter stirring for 12 h it
6. concentrationwas concentrated