HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 18961267, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 2,4-Di-tert-butylphenol | HCID 7311 | — |
| Reactant | 100304-15-2 | HCID 10998701 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 18961267 | HCID 18961267 | 78.2% |
Reaction Steps
A mixture of 20.6 g (0.10 mol) of 2,4-di-tert-butylphenol, 22.6 g (0.10 mol) of 4-carboxymethoxymandelic acid and 1 g (10 mmol) of methanesulfonic acid in 50 ml of acetic acid is refluxed for 15 hours. The acetic acid is then distilled off. The residue is dissolved in 100 ml of dichloromethane, and the solution is washed three times with water. The organic phases are combined, dried over magnesium sulfate and concentrated on a vacuum rotary evaporator. Crystallisation of the residue from ligroin gives 31.0 g (78%) of 5,7-di-tert-butyl-3-(4-carboxymethoxyphenyl)benzofuran-2-one, melting point 158°-162° C. (Compound (116), Table 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05356966 |
| Source dataset | uspto-grants-1994_10 |
| ORD ID | ord-13a59224261d4cdfa6d6ffa72df9e6e5 |
| Source note | uspto-grants-1994_10 |