Hexane → (3-Ethylcyclopentadienyl)(cyclopentadienyl)dimethylsilane

Temperature

-78 °C

Ethylcyclopentadiene in an amount of 7.52 g (80 mmol) was dissolved in 100 ml of THF, and the solution was cooled to −78° C. A 1.58 M hexane solution of n-butyllithium in a volume of 56 ml (92 mmol) was added thereto dropwise. The mixture was stirred at room temperature for 2 hours and was added dropwise to 50 ml of THF containing 110 mmol of the chloro(cyclopentadienyl)dimethylsilane at −78° C. The temperature was gradually increased, and the mixture was stirred at room temperature for 24 hours and was concentrated under reduced pressure. Insolubles were removed by filtration. The filtrate was washed with hexane and was distilled under reduced pressure. The distillate was subjected to silica gel column chromatography, and 0.86 g of (3-ethylcyclopentadienyl)(cyclopentadienyl)dimethylsilane was obtained. The compound was identified by GC-MS. GC-MS: 216 (MS).

1. temperatureThe temperature was gradually increased
2. stirringthe mixture was stirred at room temperature for 24 hours
3. concentrationwas concentrated under reduced pressure
4. customInsolubles were removed by filtration
5. washThe filtrate was washed with hexane
6. distillationwas distilled under reduced pressure

ORD record

ord-f6550c5ebc594c919d54313d748cbb4c

Source dataset

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08785574B2