HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methoxybenzyl alcohol → HCID 18449403, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methoxybenzyl alcohol | HCID 7738 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 16638331 | HCID 16638331 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18449403 | HCID 18449403 | — |
Reaction Steps
A mixture of (±)-5′-nitro-spiro[imidazolidine-4,2′-indane]-2,5-dione (1.4 g, 5.66 mmol, described in Intermediate 6), 4-methoxybenzyl alcohol (0.94 g, 6.80 mmol), diethyl azodicarboxylate (1.48 g, 8.49 mmol), and triphenylphosphine (2.23 g, 8.49 mmol) in THF (15 mL) was stirred at ambient temperature for 3 days. The solvent was removed under reduced pressure and the residue was partitioned between saturated aqueous NaHCO3 (15 mL) and CH2Cl2 (50 mL). The organic layer was dried (Na2SO4), filtered, and concentrated under reduced pressure. The crude product was purified by silica gel chromatography, eluting with a gradient of hexane:EtOAc—90:10 to 60:40, to give the title compound. MS: m/z=368 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071770B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-d450e0bc64cf4ea7a0da0cf3c22ad2c8 |
| Source note | uspto-grants-2011_12 |