Pentane → HCID 178440524, compound

Temperature

-35 °C

To a yellow solution of (tetramethylcyclopentadienyl)(propylcyclopentadienyl) zirconium dichloride [(Me4Cp)(PrCp)ZrCl2] (1.00 g, 2.47 mmol, 1.00 eq.) in dichloromethane (10 mL) was added tributyltin fluoride (1.60 g, 5.18 mmol, 2.09 eq.). The reaction quickly lightened, becoming almost colorless with a small amount of tributyltin fluoride still visible. 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 (15 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 0.88 g (96%). 1H NMR(CD2Cl2): δ0.92 (t, 3H, CH2CH2CH3), 1.55 (m, 2H, CH2CH2CH3), 1.82 (s, 6H, Me), 199 (s, 6H, Me), 2.42 (t, 2H, CH2CH2CH3), 5.93 (s, 1H, ring-H), 5.96 (br m, 2H, ring-H), 6.17 (m, 2H, ring-H). 19F NMR(CD2Cl2): δ17.5 (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 0.88 g (96%)

ORD record

ord-a0c74c0573484ad09b805975e2bd15fd

Source dataset

uspto-grants-2003_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06632901B2