HuagongsheHuagongshe Chemistry Print Report · For research reference only
Glycidol → HCID 43185732, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Glycidol | HCID 11164 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 4-nitro-1H-pyrazole | HCID 16376 | — |
| Reactant | Diisopropyl azodicarboxylate | HCID 5363146 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 43185732 | HCID 43185732 | 48% |
Reaction Steps
To a stirred, cooled (0° C.) solution of 4-nitro-1H-pyrazole (1.0 g, 8.8 mmol), glycidol (0.58 mL, 8.8 mmol) and triphenylphosphine (2.14 g, 10.6 mmol) in THF (40 mL) was added DIAD (2.25 mL, 11.4 mmol). After 24 h the reaction mixture was diluted with ethyl acetate and water. The aqueous layer was extracted with ethyl acetate and the combined organic layers were washed (brine), dried (anhydrous MgSO4) and concentrated. Flash chromatography (Isolera, silica, 50 g, 0-90% ethyl acetate in petroleum ether) afforded 4-nitro-1-(oxiran-2-ylmethyl)-1H-pyrazole as an off-white solid (0.71 g, 48% yield). LCMS (UPLC, low pH), RT=0.74 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09242987B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-164786ff434140e9a947975515c40ddd |
| Source note | uspto-grants-2016_01 |