反应详情

A solution of N-{2-[(4-butylphenyl)ethynyl]benzyl}-1-hexanamine (174 mg, 0.50 mmol), 2,2-dimethyl-4-oxo-4H-1,3-benzodioxine-6-carboxylic acid (122 mg, 0.55 mmol), EDC.HCl (115 mg, 0.60 mmol), DIEA (102 μl, 0.60 mmol) and HOBT (81 mg, 0.60 mmol) in DCM (10 mL) was stirred at rt for 3 hrs. The reaction mixture was diluted with DCM and washed with a saturated aqueous solution of NaHCO3, an aqueous solution of HCl (1N) and brine. The organic layer was dried over MgSO4 and the solvent Was removed under reduced pressure. Purification by flash chromatography on silicagel (EtOAc/c-Hex (20/80)) gave 238 mg (87%) of the title compound. HPLC, Rt: 6.14 min (purity: 86.7%).

1. washwashed with a saturated aqueous solution of NaHCO3
2. dry with materialThe organic layer was dried over MgSO4
3. customthe solvent Was removed under reduced pressure
4. customPurification by flash chromatography on silicagel (EtOAc/c-Hex (20/80))