[1,1'-Biphenyl]-3-aMine, 4,4'-difluoro- synthesis
- Product Name:[1,1'-Biphenyl]-3-aMine, 4,4'-difluoro-
- CAS Number:323-93-3
- Molecular formula:C12H9F2N
- Molecular Weight:205.2
Yield:323-93-3 65%
Reaction Conditions:
with tetrakis(triphenylphosphine) palladium(0);potassium carbonate in water;toluene; for 24 h;Reflux;
Steps:
1 Synthesis of Intermediate A-1
5.7 g (30 mmol) of 5-bromo-2-fluoroaniline, 4.2 g (30 mmol) of (4-fluorophenyl)boronic acid, 520 mg (0.45 mmol) of tetrakistriphenylphosphinopalladium (Pd(PPh3)4), and 63 ml (126 mmol) of a 2M K2CO3 aqueous solution were dissolved in 200 ml of toluene and mixed. The mixture was refluxed for 24 hours. After the reaction was completed, the solvent was removed by evaporation, 500 ml of ethylacetate and 500 ml of water were added to wash the resultant, and an organic layer was collected and dried using magnesium sulfate anhydride. Then, the resultant was purified by silica gel chromatography, and 4.0 g of Intermediate A-1 was obtained (65% yield).
References:
US2013/228752,2013,A1 Location in patent:Paragraph 0137; 0138