HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 968308Generated: October 29, 2026
Triphenylphosphine → HCID 22288647, compound
https://huagongshe.com/reaction/968308
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 15594572 | HCID 15594572 | — |
| Reactant | HCID 178516755 | HCID 178516755 | — |
| Solvent | Toluene | HCID 1140 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22288647 | HCID 22288647 | 44% |
Reaction Steps
5,6-Di(2-pyridyl)-2-pyrazinol (1.21 g), 2-[4-(1H-imidazolylmethyl)phenoxy]-1-ethanol (1.05 g), and triphenylphosphine (1.27 g) were dispersed in tetrahydrofuran (30 mL). A 40% solution (2.10 g) of diethyl azodicarboxylate in toluene was added dropwise to the dispersion under ice cooling, and the resultant mixture was allowed to react overnight, while the temperature of the mixture was gradually elevated to room temperature. After completion of reaction, ethyl acetate was added to the reaction mixture, and the ethyl acetate layer was washed with water. The washed product was dried over sodium sulfate anhydrate, and the residual solvent was removed through distillation under reduced pressure. The thus-yielded residue was purified by means of a silica gel column and recrystallized from ethyl acetate, to thereby yield 960 mg of Compound (1B) of the present invention as pale yellow crystals (yield 44.0%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06958353B2 |
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| Source dataset | uspto-grants-2005_10 |
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| ORD ID | ord-c817d518f95b4810a0e6e8f96bdb3b47 |
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| Source note | uspto-grants-2005_10 |
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