HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → Diphenyl Ether
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 69946721 | HCID 69946721 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Diphenyl Ether | HCID 7583 | 32% |
Reaction Steps
To a stirred solution of N-ethyl,N-propionyl tyramine (2.84 g, 12.83 mmole) in tetrahydrofuran (32.1 ml) was added 60% sodium hydride dispersion (0.56 g, 14.11 mmole). After stirring for 10 minutes, the compound of Example 42(E) (4.70 g, 12.83 mmole) was added. The reaction was allowed to stir at room temperature for 5 hours, poured into ethyl acetate, and extracted with 10% sodium sulfate, then brine. The organic layer was dried over sodium sulfate, evaporated to dryness, and chromatographed on silica gel using a hexane-ethyl acetate gradient. Further chromatography on silica gel using toluene-acetone gradients yielded the intermediate phenyl ether (2.10 g, 32%):
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06579871B2 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-2abccaddf4d84463ad022c9ee2a1f974 |
| Source note | uspto-grants-2003_06 |