HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → 4-Methyl-2-(3,3,5,5-tetramethylcyclohexyl)phenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 1-Methoxy-4-methyl-2-(3,3,5,5-tetramethylcyclohexyl)benzene | HCID 23142420 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 4-Methyl-2-(3,3,5,5-tetramethylcyclohexyl)phenol | HCID 23142895 | 47.6% |
Reaction Steps
To a solution of 1-methoxy-4-methyl-2-(3,3,5,5-tetramethylcyclohexyl)benzene (1.0 g, 3.84 mmol) produced in Example (104b) in acetic acid (5 mL) was added 48% hydrobromic acid (10 mL, 59.3 mmol), followed by reflux for 12 hours. Saturated aqueous solution of sodium hydrogencarbonate was added to the cooled reaction mixture, and extraction was performed with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and the filtrate was concentrated under reduced pressure to give a residue, which was purified by silica gel column chromatography (ethyl acetate/heptane) to give 450 mg of the title compound as a light yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07410971B2 |
| Source dataset | uspto-grants-2008_08 |
| ORD ID | ord-6ce7fb14ca5848b6b219ecf3a7638dc9 |
| Source note | uspto-grants-2008_08 |