참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 4,4,5,5-Tetramethyl-2-(prop-1-en-2-yl)-1,3,2-dioxaborolane | HCID 10997426 | — |
| 반응물 | Methyl 4-bromo-2-methylbenzoate | HCID 22031226 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 4-Isopropenyl-2-methyl-benzoic acid methyl ester | HCID 59216521 | 88.5% |
반응 단계
4-Bromo-2-methyl-benzoic acid methyl ester (4 g, 17.46 mmol), isopropenylboronic acid pinacol ester (3.228 g, 19.21 mmol) and cesium carbonate (19.913 g, 61.11 mmol) were treated with a degassed solution of 15 ml dioxane/5 ml water. After 5 min stirring [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) complex (0.718 g, 0.873 mmol) was added and heated to 120° C. for 40 min in the microwave. The reaction mixture was filtered over cellulose; washed with 20 ml dioxane and concentrated in vacuo. The residue was purified by 120 g silica gel chromatography (gradient elution 0-50% ethyl acetate in hexane during 50 min) to yield 4-Isopropenyl-2-methyl-benzoic acid methyl ester (2.94 g, 15.45 mmol). MS (ESI) 191.3 (M+H)+
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08536166B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-023600dfa07a48a7b0cac71e0606de8b |
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| 출처 메모 | uspto-grants-2013_09 |
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