Chlorotrimethylsilane → 1,3-Cyclopentadiene, (trimethylsilyl)-

Temperature

-78 °C

11 g of trimethylsilyl chloride was dissolved in 30 mol of well dried tetrahydrofuran in a 300 ml flask whose inside had been substituted by nitrogen, and the obtained solution was cooled to −78° C. 100 ml of a tetrahydrofuran solution (2.0 mol/l) of cyclopentadienyl sodium was added dropwise to the above solution in a stream of nitrogen over 1 hour. The solution was stirred at −78° C. for 1 hour and returned to room temperature over 6 hours. A salt precipitated in the mixture solution was removed by filtration in a nitrogen atmosphere, and the residual solution was distilled to obtain 8 g of trimethylsilyl cyclopentadiene.

1. waitreturned to room temperature over 6 hours
2. customA salt precipitated in the mixture solution
3. customwas removed by filtration in a nitrogen atmosphere
4. distillationthe residual solution was distilled

ORD record

ord-8af64c012b31467698caaf0202fc5dfe

Source dataset

uspto-grants-2007_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07238822B2