HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 6-tert-Butyl-2,2-dimethyl-2,3-dihydro-1-benzofuran-5-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 4,6-di-t-butyl-5-hydroxy-2,2-dimethyl-2,3-dihydrobenzofuran | HCID 10062026 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 6-tert-Butyl-2,2-dimethyl-2,3-dihydro-1-benzofuran-5-ol | HCID 15737520 | 41% |
Reaction Steps
To 0.28 g of 4,6-di-t-butyl-5-hydroxy-2,2-dimethyl-2,3-dihydrobenzofuran synthesized according to JP 6-206842A/94 dissolved in 5 ml of chloroform was added 0.06 ml of methanesulfonic acid and the mixture was stirred at room temperature for 4 hours. Then, the reaction mixture was combined with a saturated aqueous sodium bicarbonate solution and extracted with chloroform. The extracted layers were washed with saturated brine, dried over anhydrous magnesium sulfate and then concentrated. The concentrate was purified by silica gel column chromatography (in n-hexane containing 10% ethyl acetate) to give 0.09 g of 6-t-butyl-5-hydroxy-2,2-dimethyl-2,3-dihydrobenzofuran as a white solid (yield 41%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06403639B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-869c5e6358d24f02b8276556d3d404fe |
| Source note | uspto-grants-2002_06 |