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Reaction id: 0501011023_08, verified by Personal Chemistry ©
2-Fluoroanisole
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Phenylmagnesium ...
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Pd(dba)2
Cy2PPh
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THF
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p17
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Yield: 98% Time: 600s Temperature: 150 °C
Chemicals
| Name |
MW [g/mol] |
Density [g/ml] |
Amount [mmol] |
Mass/Volume |
| 321-28-8 |
126.130 |
1.120 |
1.036 |
116.675 µl |
| 100-59-4 (2.0M in THF) |
136.871 |
1.000 |
3.000 |
1500.000 µl |
| Pd(dba)2 |
574.996 |
1.000 |
0.054 |
30.884 mg |
| Cy2PPh |
274.388 |
1.000 |
0.107 |
29.265 mg |
| THF |
72.107 |
0.889 |
12.329 |
1000.000 µl |
| Product 1 |
184.238 |
1.000 |
0.000 |
0.000 µl |
Keywords
Catalysis, Catalyzed, Grignard Reaction, Metal
Comments
Synthesis: In this article, a number of nickel and palladium catalysts and phosphine ligands were tried out for the Grignard reaction of aryl fluorides and aryl magnesium chlorides. The best catalyst/ligand combinations were found to be Nickel(II) acetylacetonate with tris(2,4-di-tert-butylphenyl) phosphite or tris(4-(Dimethylamino)phenyl)phosphine and, for palladium catalysed reactions, bis(dibenzylideneacetone)palladium(0) with dicyclohexylphenylphosphine. No inert atmosphere was needed for these microwave reactions.
Work-up and analysis: To the reaction mixture was added an internal standard (tridecane). After heating, the reaction mixture was poured into 0.5 M aqueous HCl and the extracted with 3*10 ml MTBE. GCMS analysis of the organic phase was used to determine the reaction yield.
Instrument Settings
Absorption level: Normal
Pre-stirring time: 0s
References
Dankwardt, J. W. J. Organomet. Chem. 2004, 690, 4, 932-938
Analysis
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