HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 18348567, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 3,4,5-Trimethoxyphenol | HCID 69505 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | 7-(2-Hydroxyethyl)-2,3-dimethoxy-4,5,6,7,8,9-hexahydro-1H-benzo[a]cycloheptene-1,4-dione | HCID 18348573 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18348567 | HCID 18348567 | 79.9% |
Reaction Steps
To a solution of 7-(2-hydroxyethyl)-2,3-dimethoxy-4,5,6,7,8,9-hexahydro-1H-benzo[a]cycloheptene-1,4-dione (165 mg), 3,4,5-trimethoxyphenol (335 mg), and triphenylphosphine (201 mg) in THF (3 ml) was added a solution of diethyl azodicarboxylate (148 mg) in THF (1 ml) at room temperature. The reaction mixture was stirred at room temperature for 25 min and concentrated. The residue was purified by alumina column chromatography (eluent: ethyl acetate/hexane=1/4) and with recrystallization from ethyl acetate-hexane to obtain the entitled compound (210 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06326369B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-f93a2c5b1ff047d8894119e9ca3275da |
| Source note | uspto-grants-2001_12 |