HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-Methoxy-3-isochromanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| Reactant | Ethyl alpha-methoxy-2-(tetrahydropyran-2-yloxymethyl)phenylacetate | HCID 18357803 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 4-Methoxy-3-isochromanone | HCID 15547285 | 74.2% |
Reaction Steps
Pyridinium p-toluenesulfonate (0.30 g) was added to a solution of ethyl α-methoxy-2-(tetrahydropyran-2-yloxy-methyl)phenylacetate (14.00 g, 45.4 mmol) in methanol (50 ml), and the mixture was heated under reflux for 1 hour. The mixture was cooled to room temperature, and water (50 ml) was added. The mixture was extracted with methylene chloride and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the residue was purified by recrystallization from n-hexane/ethyl acetate (=1/1) to give the desired compound 4-methoxy-3-isochromanone (6.00 g, 74.2%) as white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05948819 |
| Source dataset | uspto-grants-1999_09 |
| ORD ID | ord-5f8fd03e8b974d4cb63bfdc7c3fcf2fc |
| Source note | uspto-grants-1999_09 |