HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → 4-Isopropenyl-2-methyl-benzoic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 4,4,5,5-Tetramethyl-2-(prop-1-en-2-yl)-1,3,2-dioxaborolane | HCID 10997426 | — |
| Reactant | Methyl 4-bromo-2-methylbenzoate | HCID 22031226 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 4-Isopropenyl-2-methyl-benzoic acid methyl ester | HCID 59216521 | 88.5% |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
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)+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08324211B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-875422ee8b444a88a8351ea0929957e8 |
| Source note | uspto-grants-2012_12 |