HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 67966896, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 67958076 | HCID 67958076 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67966896 | HCID 67966896 | 98.7% |
Reaction Steps
To a solution of 2-[2-(hydroxymethyl)-2-methylcyclopropyl]-3-{[(methyloxy)methyl]oxy}phenol (Intermediate 123, 307 mg) in dry tetrahydrofuran (10 ml) were added triphenylphosphine (338 mg, 1.288 mmol) and bis(1-methylethyl)(E)-1,2-diazenedicarboxylate (261 mg, 1.288 mmol). The reaction turned yellow and was stirred for 20 minutes at room temperature under nitrogen. The solvent was then evaporated under vacuum to give the crude product as pale yellow oil. The residue obtained was purified by silica gel chromatography (Companion system, with a gradient from pure Cyclohexane to cyclohexane/ethyl acetate 10/1) to give the title compound as a white solid (280 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09346790B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-4bbcd25fe46c480c9b891d482a698c8c |
| Source note | uspto-grants-2016_05 |