Toluene → Aluminum, triphenyl-

To a suspension of AlCl3 (1.25 g, 9.4 mmol) in diisopropyl ether (20 mL) was added phenylmagnesium bromide (10.8 mL, 27 mmol, 2.5 M in Et2O) at 0-5° C. The mixture was stirred at room temperature for 3-4 hours. The solvent was removed using a high-vacuum pump affording a white solid. To the solid was added PhMe (15 mL) and the mixture was stirred for 15 min, and then the resulting slurry was filtered under an atmosphere of nitrogen. The clear filtrate was evaporated to about ⅓rd of the original volume and the resulting solid was filtered affording 1.36 g of crude product. A slurry of the crude product and PhMe (15 mL) was stirred, and was then filtered. The filtrate was evaporated to about ⅓rd of the original volume and the resulting solid was filtered affording the desired product (0.56 g, 18%).

1. customThe solvent was removed
2. customaffording a white solid
3. stirringthe mixture was stirred for 15 min
4. filtrationthe resulting slurry was filtered under an atmosphere of nitrogen
5. customThe clear filtrate was evaporated to about ⅓rd of the original volume
6. filtrationthe resulting solid was filtered
7. customaffording 1.36 g of crude product
8. filtrationwas then filtered
9. customThe filtrate was evaporated to about ⅓rd of the original volume
10. filtrationthe resulting solid was filtered

ORD record

ord-f53bc8737fc04d9f91cc3d2551609184

Source dataset

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08952139B2