Sodium Carbonate → HCID 86708422, compound

Participants

Reaction Conditions

Reaction Steps

Under a nitrogen atmosphere, potassium hydride (0.88 g, 21.82 mmol in terms of potassium hydride) dispersed in mineral oil was washed with hexane. Tetrahydrofuran (38 mL) was added and this mixture was warmed to 50° C. A solution of 1,2,3,4-tetramethylcyclopenta-1,3-diene (2.00 g, 16.37 mmol) dissolved in tetrahydrofuran (8 mL) was added dropwise and stirred at 50° C. for one hour. To this solution, a solution of chlorotris(5-methyl-3-trimethylsilyl-phenyl)silane (7.81 g, 14.11 mmol) dissolved in tetrahydrofuran (38 mL) was added dropwise and stirred at 65° C. for 3 hours. The resultant mixture was added dropwise at 0° C. to a solution of a 10% sodium hydrogen carbonate (38 mL) and a 10% sodium carbonate (38 mL). Toluene (38 mL) was added to separate an organic phase, and the organic phase was dried over sodium sulfate and then filtrated. The solvent was removed under reduced pressure. Purification was performed by silica gel column chromatography to obtain 1-tris(5-methyl-3-trimethylsilyl-phenyl)silyl-2,3,4,5-tetramethylcyclopentadiene (5.40 g, yield 59.9%).

Provenance & Evidence