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HRID 130647作成日:2026年10月27日

Dimethyl dicarbonate → 2,3,3',4'-Tetramethylbenzophenone

https://huagongshe.com/reaction/130647

反応式

関与物質

役割名称HCID仕込み量
反応物Dimethyl dicarbonateHCID 3086—
反応物Potassium CarbonateHCID 11430—
反応物3,4-Dimethylbenzoic acidHCID 12073—
反応物2,3-Dimethylphenylboronic acidHCID 2773395—
触媒PalladiumHCID 23938—
溶媒WaterHCID 962—
溶媒1,4-DioxaneHCID 31275—
生成物2,3,3',4'-TetramethylbenzophenoneHCID 2037211842%

反応条件

温度80 °C

反応手順

To a 250 ml 3-necked round-bottom flask, 2,3-dimethylphenylboronic acid (3.6 g. 24 mmol). 3,4-dimethylbenzoic acid (3.0 g. 20 mmol), a selected palladium catalyst (0.6 mmol), dimethyl dicarbonate (2.7 g. 30 mmol) and potassium carbonate (6.22 g. 45 mmol) were mixed with 150 ml of dry dioxane. The reaction mixture was heated at 80° C. overnight to become a viscous reaction mixture. 20 ml of water was added to dissolve the heterogeneous reaction mixture, and dioxane was evaporated to dryness. The aqueous solution was extracted with 20 ml of ethyl acetate, dried over anhydrous magnesium sulfate and then evaporated to dryness. The crude product was purified by silica gel column chromatography eluted by hexane/ethyl acetate=20/80 to afford 2.0 g (33%) of the product.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07381849B1
出典データセットuspto-grants-2008_06
ORD IDord-3be3222c0dbc41d1af544c056c2c0c43
出典メモuspto-grants-2008_06