HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 69020207, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Di-tert-butyl azodicarboxylate | HCID 97268 | — |
| Reactant | HCID 67211053 | HCID 67211053 | — |
| Reactant | HCID 178437439 | HCID 178437439 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 69020207 | HCID 69020207 | 39.6% |
Reaction Steps
[step 1] (E)-(3-Hydroxymethyl-6,11-dihydrodibenzo[b,e]oxepin-11-ylidene)acetonitrile (JP-B-2526005; 250 mg, 0.950 mmol) and 2-ethyl-5,7-dimethyl-3H-imidazo[4,5-b]pyridine (250 mg, 1.42 mmol) were dissolved in THF (9.5 mL), and the solution was added with polymer supported triphenylphosphine (633 mg, 1.90 mmol) and di-t-butyl azodicarboxylate (437 mg, 1.90 mmol) at 0° C., followed by stirring at room temperature for 3 hr. The mixture was filtrated and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=1/1) to give (E)-[3-(2-ethyl-5,7-dimethyl-3H-imidazo[4,5-b]pyridin-3-yl)methyl-6,11-dihydrodibenzo[b,e]oxepin-11-ylidene]acetonitrile (158 mg, 26%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08242151B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-3b81285a72c4481a986e50446f16d966 |
| Source note | uspto-grants-2012_08 |