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HRID 661770作成日:2026年10月25日

Sodium Carbonate → HCID 69230364、化合物

https://huagongshe.com/reaction/661770

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium CarbonateHCID 10340—
反応物Potassium hydrideHCID 82127—
反応物Sodium BicarbonateHCID 516892—
反応物3,6-DI-Tert-butylfluoreneHCID 11140437—
反応物(2-Allyloxy-3-tert-butyl-5-methylphenyl)chlorodiethylsilaneHCID 67206735—
溶媒TolueneHCID 1140—
溶媒TetrahydrofuranHCID 8028—
溶媒HexaneHCID 8058—
生成物HCID 69230364HCID 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

DOI10.6084/m9.figshare.5104873.v1
特許番号US08084559B2
出典データセットuspto-grants-2011_12
ORD IDord-292c8949cf154008a7589145cc64c0e7
出典メモuspto-grants-2011_12