참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethyl dicarbonate | HCID 3086 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3,4-Dimethylbenzoic acid | HCID 12073 | — |
| 반응물 | 2,3-Dimethylphenylboronic acid | HCID 2773395 | — |
| 촉매 | Palladium | HCID 23938 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 2,3,3',4'-Tetramethylbenzophenone | HCID 20372118 | 42% |
반응 단계
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 as 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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08093348B1 |
|---|
| 출처 데이터셋 | uspto-grants-2012_01 |
|---|
| ORD ID | ord-40f67c7c6ebe4f6fa1f0e5363b4b4569 |
|---|
| 출처 메모 | uspto-grants-2012_01 |
|---|