Pentane → HCID 178440522, compound

Temperature

-35 °C

To a straw yellow solution of bis(propylcyclopentadienyl) zirconium dichloride [(PrCp)2ZrCl2] (1.00 g, 2.66 mmol, 1.00 eq.) in dichloromethane (10 mL) was added tributyltin fluoride (1.72 g, 5.57 mmol, 2.10 eq.). The reaction rapidly lightened, turning almost colorless. The reaction was stirred 1 h and was then filtered to give a colorless solution and a small amount of white solid. The solution was evaporated in vacuo, leaving a damp, white solid. Pentane (10 mL) was added and the mixture was cooled to −35° C. The mixture was filtered, and resulting white solid was washed with pentane (3×3 mL) cooled to −35° C. The white solid was dried in vacuo to yield 0.75 g (82%). 1H NMR(CD2Cl2): δ 0.92 (t, 6H, CH2CH2CH3), 1.56 (m, 4H, CH2CH2CH3), 2.44 (t, 4H, CH2CH2CH3), 6.05 (m, 4H, ring-H), 6.30 (m, 4H, ring-H). 19F NMR(CD2Cl2): δ 20.4 (s).

1. customThe reaction
2. filtrationwas then filtered
3. customto give a colorless solution
4. customThe solution was evaporated in vacuo
5. customleaving a damp, white solid
6. filtrationThe mixture was filtered
7. customresulting white solid
8. washwas washed with pentane (3×3 mL)
9. temperaturecooled to −35° C
10. customThe white solid was dried in vacuo
11. customto yield 0.75 g (82%)

ORD record

ord-a47443a3afa24c9d90c385c0cb0e18dd

Source dataset

uspto-grants-2006_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07132382B2