HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,3-Dihydro-1-benzofuran-4-carboxylic acid → (2,3-Dihydro-1-benzofuran-4-yl)methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,3-Dihydro-1-benzofuran-4-carboxylic acid | HCID 18787444 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (2,3-Dihydro-1-benzofuran-4-yl)methanol | HCID 18787415 | — |
Reaction Steps
A solution of 2,3-dihydrobenzofuran-4-carboxylic acid (10 g, 61 mmol) in THF (100 mL) was stirred as LAH (4.64 g, 122 mmol) was slowly added. The mixture was heated to reflux for 30 min. The mixture was cooled and quenched cautiously with ethyl acetate and then with 1N HCl (150 mL). The mixture was then made acidic with 12N HCl until all the inorganic precipitate dissolved. The organic layer was separated, and the inorganic layer was extracted twice with ethyl acetate. The organic layers were combined, washed twice with brine, and then concentrated in vacuo. This oil was Kugelrohr distilled to a clear oil that crystallized upon cooling (8.53 g, 87.6%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05856529 |
| Source dataset | uspto-grants-1999_01 |
| ORD ID | ord-4f22dd669dd2413cb635917ab11aed17 |
| Source note | uspto-grants-1999_01 |