反应详情

Trans-2-(4-Chloro-benzenesulfonylamino)-cyclohexanecarboxylic acid (0.095 g, 0.3 mmol) is dissolved in CH3CN. O-1,2-Dihydro-2-oxo-1-pyridyl)-N,N,N′,N′-tetramethyluronium tetrafluoroborate (TPTU, 90.2 mg, 0.3 mmol), N-Ethyldiisopropylamine (DIPEA, 0.208 ml, 1.21 mmol) are added. The amino-(3-hydroxy-phenyl)-acetonitrile in CH3CN (1.5 ml) is added. The mixture is stirred at RT for 16 hours. The solution is filtered and concentrated. The residue is dissolved in CH2Cl2 (15 mL) and extracted with NH4Cl (2×10 ml). The H2O layers are extracted with CH2Cl2 (2×15 ml). The collected CH2Cl2 layers are dried over MgSO4 and evaporated. The solid is purified by preparative HPLC.

1. filtrationThe solution is filtered
2. concentrationconcentrated
3. dissolutionThe residue is dissolved in CH2Cl2 (15 mL)
4. extractionextracted with NH4Cl (2×10 ml)
5. extractionThe H2O layers are extracted with CH2Cl2 (2×15 ml)
6. dry with materialThe collected CH2Cl2 layers are dried over MgSO4
7. customevaporated
8. customThe solid is purified by preparative HPLC