HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 17860745, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pivaloyl chloride | HCID 62493 | — |
| Reactant | 5-Hydroxy-1-tetralone | HCID 119921 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 17860745 | HCID 17860745 | — |
Reaction Steps
To a pyridine (180 ml) solution of 5-hydroxy-1-tetralone (30.0 g), 4-dimethylaminopyridine (1.13 g) was added, and pivaloyl chloride (25.0 ml) was added thereto under ice-cooling, followed by stirring at room temperature overnight. The reaction mixture was ice-cooled, and a concentrated hydrochloric acid was added thereto, followed by extracting with ethyl acetate. The extract was washed with water and saturated saline in this order, dried with anhydrous magnesium sulfate, and concentrated. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1 to 5:1) to thereby obtain the title compound (45.4 g) having the following physical data.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07220864B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-7e275e88ec1d4ac483d6f2fc83a9160a |
| Source note | uspto-grants-2007_05 |