反应详情

To a solution of 1,1-dimethyl Tic (240 mg, 1.17 mmol), 4-Cl-D-Phe-OMe (322 mg, 1.28 mmol), HOBT (197 mg, 1.46 mmol), and DIPEA (0.81 mL, 44.68 mmol) in DCM/DMF (1:1) was added EDC (280 mg, 1.46 mmol). The resulting mixture was stirred at r.t. overnight. The mixture was then diluted with EtOAc (100 mL), washed with saturated aqueous NaHCO3 and brine, and then dried (Na2SO4) and concentrated to dryness. Purification and separation of diastereomers by flash chromatography (35 g SiO2, linear gradient, 40 mL/min 10–50% EtOAc/hexane for 25 minutes and 50% EtOAc/hexane for 7 minutes) afforded the final compound. LRMS (ESI+): 401.1 (M+H)

1. washwashed with saturated aqueous NaHCO3 and brine
2. dry with materialdried (Na2SO4)
3. concentrationconcentrated to dryness
4. customPurification and separation of diastereomers by flash chromatography (35 g SiO2, linear gradient, 40 mL/min 10–50% EtOAc/hexane for 25 minutes and 50% EtOAc/hexane for 7 minutes)