Water → HCID 54565416, compound

1,2,3-Trimethylindene in an amount of 4.09 g (26 mmol) was dissolved in 100 mL of dried THF, and to the resultant solution was added dropwise, under ice-cooling 19 mL of a 1.7M solution of tert-butyllithium in pentane. After 2 hours of reaction at room temperature, the reaction product was incorporated under ice-cooling with 3.25 g (30 mmol, 3.8 mL) of trimethylchlorosilane (TMSCl) that had been subjected to simple distillation, was brought back to room temperature and was allowed to stand overnight. The yellow solution thus obtained was incorporated with 20 mL of water for quenching and THF was removed under reduced pressure. Then, the solution was extracted and separated with 300 mL of hexane, the organic phase thus obtained was dried with magnesium sulfate anhydride as the drying agent, the used drying agent was filtered away, and the volatile components were distilled away under reduced pressure. As the result, there was produced 1,2,3-trimethylindenyltrimethylsilane in the form of yellow oil in a yield of 4.27 g (18.5 mmol) and in a yield rate of 72%.

1. customAfter 2 hours of reaction at room temperature
2. distillationhad been subjected to simple distillation
3. customwas brought back to room temperature
4. customThe yellow solution thus obtained
5. customfor quenching
6. customTHF was removed under reduced pressure
7. extractionThen, the solution was extracted
8. customseparated with 300 mL of hexane
9. customthe organic phase thus obtained
10. dry with materialwas dried with magnesium sulfate anhydride as the drying agent
11. customthe used drying agent
12. filtrationwas filtered away
13. distillationthe volatile components were distilled away under reduced pressure

ORD record

ord-40a5d4a72e1a49af8ec50e432125ee9a

Source dataset

uspto-grants-1998_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05747614