Sodium Carbonate → HCID 123427119, compound

Participants

Reaction Conditions

Reaction Steps

Under a nitrogen atmosphere, to potassium hydride dispersed in mineral oil (1.19 g, 29.78 mmol in terms of potassium hydride), tetrahydrofuran (108 mL) was added. This mixture was warmed to 50° C. and a solution of 1,2,3,4-tetramethylcyclopenta-1,3-diene (2.73 g, 22.34 mmol) dissolved in tetrahydrofuran (27 mL) was added dropwise. Stirring was performed at 50° C. for 1 hour. To this solution, a solution of chlorotris{3,5-bis(trimethysilyl)phenyl}silane (13.55 g, 18.62 mmol) dissolved in tetrahydrofuran (27 mL) was added dropwise and stirred at 50° C. for 5 hours. The resultant mixture was added dropwise at 0° C. to a solution of 10% sodium hydrogen carbonate (68 ml) and 10% sodium carbonate (68 mL). Toluene (68 mL) was added to separate an organic phase. After dried over sodium sulfate, the organic phase was filtrated. The solvent was removed under reduced pressure. Hexane was added and the obtained white solid was filtrated to obtain 1-tris{3,5-bis(trimethylsilyl)phenyl}silyl-2,3,4,5-tetramethylcyclopentadiene (7.01 g, yield 46.2%).

Provenance & Evidence