Water → HCID 178494847, compound

A solution of 4.5 g (37.7 mmol) 2-methoxyethylcyclopentadiene in 50 ml THF was added to 2.20 g (58.0 mmol) clean, dry potassium metal under nitrogen. This was stirred for two hours at room temperature and warmed to 40 20 C. for a further two hours. After cooling, the solution was filtered and the remaining potassium washed, dried and weighed. The yield of potassium 2-methoxyethylcyclopentadienylide (KCp*) was calculated to be 4.20 g (26.4 mmol). The KCp* solution was added to a slurry of 3.03 g (13.0 mmol) zirconium tetrachloride in 20 ml THF and stirred for two hours. Approximately 0.5 ml water was added to the reaction vessel and the volatiles removed under reduced pressure. The residue was extracted with diethyl ether and filtered. The volume of ether was reduced under vacuum until precipitation began. Cooling to -50° C. in a low temperature freezer yielded 3.50 g of product as colourless needles (8.58 mmol, 66.0%), shown to be spectroscopically pure by 1H NMR.

1. temperaturewarmed to 40 20 C
2. waitfor a further two hours
3. temperatureAfter cooling
4. filtrationthe solution was filtered
5. washthe remaining potassium washed
6. customdried
7. stirringstirred for two hours
8. customthe volatiles removed under reduced pressure
9. extractionThe residue was extracted with diethyl ether
10. filtrationfiltered
11. customThe volume of ether was reduced under vacuum until precipitation
12. temperatureCooling to -50° C. in a low temperature freezer

ORD record

ord-4201c6ca7f1e4b77988fdcc9352c36e0

Source dataset

uspto-grants-1998_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05814574