Hexane → HCID 131731675, compound

Temperature

-78 °C

THF in a volume of 100 ml was added to 6 g (49 mmol) of n-butylcyclopentadiene, and the mixture was cooled to −78° C. A 1.65 M hexane solution of n-butyllithium in a volume of 29.6 ml (48.8 mmol) was added thereto dropwise. The mixture was stirred at room temperature for 2 hours and was cooled again to −78° C. Dichloro(chloromethyl)(methyl)silane in an amount of 8.0 g (49 mmol) dissolved in 50 ml of THF was added dropwise. The mixture was stirred at room temperature for 3 hours and was concentrated under reduced pressure. Hexane was added, and the mixture was filtered. The filtrate was distilled under reduced pressure to give 3.43 g of target chloro(chloromethyl) (cyclopentadienyl)(methyl) silane.

1. temperaturewas cooled again to −78° C
2. additionwas added dropwise
3. stirringThe mixture was stirred at room temperature for 3 hours
4. concentrationwas concentrated under reduced pressure
5. additionHexane was added
6. filtrationthe mixture was filtered
7. distillationThe filtrate was distilled under reduced pressure

ORD record

ord-86f6b727bd354f08817627b70a62346d

Source dataset

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08785574B2