反应详情

温度

80 °C

Add 4-bromophenyl boronic acid (5.0 g, 24.82 mmol), tetrakis(triphenylphosphine) palladium (0) (0.717 g, 0.620 mmol) and 2 M Na2CO3 (10 mL) to a solution of 2-iodoaniline (4.5 g, 20.69 mmol) in toluene (2 mL):ethanol (20 mL), deoxygenate and heat at 80° C. under nitrogen. After 4 h, add water and extract with EtOAc. Combine the organic layers, dry over sodium sulfate, filter and concentrate under reduced pressure to give a residue. Purify the residue by flash chromatography (Silica gel-EtOAc/hexane 1:12), to provide 4′-bromo-biphenyl-2-ylamine (3.53 g, 69%). MS (m/e): 248 (M+1); 249 (M+2).

1. customethanol (20 mL), deoxygenate
2. additionadd water
3. extractionextract with EtOAc
4. dry with materialdry over sodium sulfate
5. filtrationfilter
6. concentrationconcentrate under reduced pressure
7. customto give a residue
8. customPurify the residue by flash chromatography (Silica gel-EtOAc/hexane 1:12)