関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Potassium hydride | HCID 82127 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 3,6-DI-Tert-butylfluorene | HCID 11140437 | — |
| 反応物 | (2-Allyloxy-3-tert-butyl-5-methylphenyl)chlorodiethylsilane | HCID 67206735 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | HCID 69230364 | HCID 69230364 | — |
反応手順
There was washed 1.50 g (11.22 mmol) of potassium hydride having a purity of 30% by weight with each 3 mL of hexane three times in an atmosphere of nitrogen, and 18 mL of THF was added thereto. To the obtained THF slurry of potassium hydride, 2.50 g (8.98 mml) of 3,6-di-tert-butylfluorene was added dropwise at 0° C. using 18 mL of a THF solution thereof. The obtained mixture was stirred for 2 hours at a room temperature, and then 2.92 g (8.98 mmol) of (2-allyloxy-3-tert-butyl-5-methylphenyl)chlorodiethylsilane was added dropwise at −78° C. using 4 mL of a toluene solution thereof. The temperature of the obtained liquid reaction mixture was raised up to a room temperature, and the mixture was stirred for 2 hours. The mixture was added dropwise at 0° C. to a mixture of 18 mL of a 10% aqueous solution of sodium hydrogen carbonate and 18 mL of a 10% aqueous solution of sodium carbonate, and the resultant mixture was extracted with 10 mL of toluene. The obtained extract was dried over sodium sulfate, and dried extract was concentrated under a reduced pressure, thereby obtaining quantitatively (2-allyloxy-3-tert-butyl-5-methylphenyl)(3,6-di-tert-butylfluoren-9-yl)diethylsilane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08084559B2 |
|---|
| 出典データセット | uspto-grants-2011_12 |
|---|
| ORD ID | ord-292c8949cf154008a7589145cc64c0e7 |
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| 出典メモ | uspto-grants-2011_12 |
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