HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → (2,2-dimethyl-2H-chromen-6-yl)boronic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triisopropyl borate | HCID 21531 | — |
| Reactant | 6-Bromo-2,2-dimethyl-2H-chromene | HCID 11770533 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (2,2-dimethyl-2H-chromen-6-yl)boronic acid | HCID 17750385 | 82% |
Reaction Steps
To a solution of 6-bromo-2,2-dimethyl-2H-chromene (18 g) in tetrahydrofuran (150 mL) was added butyllithium (53 mL, 1.6 M hexane solution) at −78° C. under an argon atmosphere, and the mixture was stirred for 30 min. Triisopropyl borate (21 mL) was added, and the mixture was stirred for 3 hr while allowing to warm to room temperature. 1 M hydrochloric acid (150 mL) was added to the reaction mixture, and the mixture was stirred for 2 hr and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate, and the solvent was evaporated. The residue was purified by silica gel column chromatography to give the title compound (13 g, 82%) as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07803940B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-e4a9942df8f1439a8805d772f1b2c1d6 |
| Source note | uspto-grants-2010_09 |