HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4-Bromo-2-(3-hydroxy-1,1,3-trimethyl-butyl)-phenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 2H-1-Benzopyran-2-one, 6-bromo-3,4-dihydro-4,4-dimethyl- | HCID 22568923 | — |
| Reactant | HCID 178418443 | HCID 178418443 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | 4-Bromo-2-(3-hydroxy-1,1,3-trimethyl-butyl)-phenol | HCID 22568810 | 100% |
Reaction Steps
A solution of 6-bromo-4,4-dimethyl-chroman-2-one (1 g, 3.92 mmol) in anhydrous tetrahydrofuran (20 mL) was treated with 3M solution of ethyl magnesium bromide (2.6 mL) and stirred at ambient temperature for 2 hours. The reaction mixture was poured into cold dilute hydrochloric acid and extracted with ethyl acetate (×2). The combined organic extract was dried over anhydrous sodium sulfate, filtered and evaporated in vacuo to afford a residue which was subjected to flash column chromatography over silica gel (230-400 mesh) using 10% ethyl acetate in hexane as the eluent to afford the title compound as a pale yellow solid (1.1 g, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06713647B2 |
| Source dataset | uspto-grants-2004_03 |
| ORD ID | ord-a14d312a56a641c18f4e7ea6b15245b9 |
| Source note | uspto-grants-2004_03 |