反应详情

温度

90 °C

To a solution of 4-bromo-2-chloro-N,N-diethylbenzamide from Example 23, Part A (3.10 g, 10.67 mmol) in 50 mL of DMF was added potassium carbonate (3.68 g, 26.7 mmol) and dimethyl zinc (8.0 mL of a 2.0 M solution in toluene, 16.0 mmol). The solution was degassed with a stream of argon and then there was added [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium (II) complex with dichloromethane (1:1) (175 mg, 0.21 mmol). The reaction mixture was allowed to stir at 90° C. for 18 h. The reaction mixture was allowed to cool and was diluted with ethyl acetate. The organics were washed with water and brine, dried (MgSO4) and concentrated. The residue was purified (ISCO, elution with 0-50% EtOAc/hexane, 30 min) to afford 2.15 g (90%) of the title compound as a colorless oil. LRMS (ESI): 226.2/228.2 (M+H)+.

1. customThe solution was degassed with a stream of argon
2. temperatureto cool
3. washThe organics were washed with water and brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customThe residue was purified
7. wash(ISCO, elution with 0-50% EtOAc/hexane, 30 min)