HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 66643749, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | (5-Methyl-3-pyridin-2-yl-isoxazol-4-yl)-methanol | HCID 66643722 | — |
| Reactant | HCID 178498598 | HCID 178498598 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66643749 | HCID 66643749 | 30% |
Reaction Steps
To a stirred solution of 5-hydroxy-2-methyl-2H-pyrazole-3-carboxylic acid methyl ester (355 mg, 2.28 mmol) and (5-methyl-3-pyridin-2-yl-isoxazol-4-yl)-methanol (432 mg, 2.28 mmol) in THF (10 mL) at 5° C. under argon was added triphenylphosphine (775 mg, 2.95 mmol), then diethyl azodicarboxylate (515 mg, 2.95 mmol) was added dropwise. The reaction mixture was warmed to room temperature overnight. Then the reaction mixture was evaporated and purified by chromatography (silica, heptane:ethyl acetate=1:1 to 7.5:2.5) to afford the title compound (220 mg, 30%) as a white solid. MS: m/e=329.3 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08163728B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-6176fc202079455994dfca0d9101844a |
| Source note | uspto-grants-2012_04 |