HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethyl phosphite → Tetraethyl [[2,2'-bipyridine]-4,4'-diylbis(methylene)]bis(phosphonate)
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethyl phosphite | HCID 31215 | — |
| Reactant | 4,4'-Bis(chloromethyl)-2,2'-bipyridyl | HCID 10562811 | — |
| Solvent | Methylenechloride Hexane | HCID 21226440 | — |
| Product | Tetraethyl [[2,2'-bipyridine]-4,4'-diylbis(methylene)]bis(phosphonate) | HCID 46911978 | — |
Reaction Steps
Compound 5 (2.6 g, 10.3 mmol) was refluxed overnight under N2 in triethylphosphite (50 ml). Excess P(OEt)3 was evaporated and the resulting brown oil was column chromatographed (Al2O3, CH2Cl2/MeOH: 98/2). The yellow oil thus obtained was dissolved in a mixture of CH2Cl2/hexane (1/50 ml) and let stand in the freezer to afford after filtration 4 g (85%) of compound 6 as a slightly yellow crystalline solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07932404B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-06c8ab942aeb4256b202b25ffc42d47b |
| Source note | uspto-grants-2011_04 |