反应详情

A degassed mixture of ethyl 5-chloro-2-iodobenzoate (0.621 g, 2.00 mmol), Pd(PPh3)4 (0.116 mg, 0.1 mmol), dimethoxyethane (20 mL), phenylboronic acid (0.268 g, 2.2 mmol), K2CO3 (0.829 g, 6.0 mmol), and water (5 mL) was heated under reflux for 6 h. Solvent was removed under reduced pressure. The residue was diluted with sat. NH4Cl (15 mL) and extracted with EtOAc (2×30 mL). The combined organic layers were dried (MgSO4) and concentrated. The crude product was purified by chromatography to afford ethyl 5-chloro-2-phenylbenzoate (0.473 g, 91%) as colorless oil. MS (ESI) m/z: 261.0 (M+H+).

1. temperaturewas heated
2. temperatureunder reflux for 6 h
3. customSolvent was removed under reduced pressure
4. additionThe residue was diluted with sat. NH4Cl (15 mL)
5. extractionextracted with EtOAc (2×30 mL)
6. dry with materialThe combined organic layers were dried (MgSO4)
7. concentrationconcentrated
8. customThe crude product was purified by chromatography