HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenol → HCID 18348569, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenol | HCID 996 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| 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 18348569 | HCID 18348569 | 61.3% |
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 (100 mg), phenol (109 mg), and triphenylphosphine (127 mg) in THF (2 ml) was added a solution of diethyl azodicarboxylate (82 mg) in THF (1 ml) at room temperature. The reaction mixture was stirred at room temperature for 140 min and concentrated. The residue was purified by alumina column chromatography (eluent:ethyl acetate/hexane=1/10) and then with recrystallization from ethyl acetate-hexane to obtain the entitled compound (78 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06326369B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-072423f7208f487b8ca2b5abb49e33af |
| Source note | uspto-grants-2001_12 |