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 2hours. 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 | US06603019B2 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-5638ca747ccc471cad482618d403e04d |
| Source note | uspto-grants-2003_08 |