反应详情

To a solution of 2-[5-[[tert-butyl(dimethyl)silyl]oxymethyl]-2-thienyl]acetic acid (995 mg, 3.48 mmol) in dichloromethane (40 mL) was added (S)-3,5-dichloro-4-(2-(3,4-dimethoxyphenyl)-2-hydroxyethyl)pyridine 1-oxide (1.43 g, 4.17 mmol), followed by 4-(dimethylamino)-pyridine (212 mg, 1.74 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (1.33 g, 6.96 mmol). The resultant solution was stirred at room temperature for 72 h. The reaction solution was washed with saturated aqueous sodium bicarbonate (2×30 mL), the organic phase passed through a hydrophobic frit and concentrated in vacuo. The residue was purified by silica gel chromatography, eluting with 0-100% ethyl acetate in iso-hexane to give the title compound as a pale yellow oil (980 mg, 46%).

1. washThe reaction solution was washed with saturated aqueous sodium bicarbonate (2×30 mL)
2. concentrationconcentrated in vacuo
3. customThe residue was purified by silica gel chromatography
4. washeluting with 0-100% ethyl acetate in iso-hexane