反应详情

温度

160 °C

From a related procedure (Helv. Chim. Acta, 2004, 87, 825) a mixture of methyl 4-bromobenzoate (676 mg, 3.14 mmol), anhydrous NiBr2 (34.3 mg, 0.157 mmol), and PhP(OMe)2 (0.500 mL, 3.14 mmol) was added to a pressure vessel and heated to 160° C. (oil bath temperature) for 2 h. The reaction was cooled, diluted with EtOAc and washed with water (3×), brine, dried (MgSO4) and concentrated to afford ˜800 mg of a clear, colorless oil that solidified upon standing. The product was purified by MPLC (15-50% EtOAc in CH2Cl2) to afford the requisite product: MS: cal'd 291 (MH+), exp 291 (MH+).

1. additionwas added to a pressure vessel
2. temperatureThe reaction was cooled
3. washwashed with water (3×), brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customto afford ˜800 mg of a clear, colorless oil that
7. customThe product was purified by MPLC (15-50% EtOAc in CH2Cl2)
8. customto afford the requisite product