HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 18397192, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | ethyl N-ethoxycarbonyliminocarbamate | HCID 220568 | — |
| Reactant | HCID 22857780 | HCID 22857780 | — |
| Reactant | 2-(2,3-Difluoro-4-hydroxyphenyl)-5-(6-octyloxypyridin-3-yl)pyrimidine | HCID 135597445 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18397192 | HCID 18397192 | 87.5% |
Reaction Steps
3.2 mmol of diethyl azodicarboxylate are added dropwise at 0° C. to 3.2 mmol of triphenylphosphine in 20 ml of THF, and the mixture is stirred at room temperature for a further 20 minutes. 2.4 mmol of 2-(2,3-difluoro-4-hydroxyphenyl)-5-(6-octyloxypyridin-3-yl)pyrimidine and 2.4 mmol of 2-(S)-fluorodecanol are then added, and the reaction mixture is allowed to stand overnight. After the solvent has been removed in vacuo, the crude product is chromatographed on silica gel 60 using dichloromethane/ethyl acetate 20:1 (v/v) as eluent and is recrystallized from acetonitrile, giving 1.2 g (86%) of colorless crystals, X 97 SC * 150.5 SA 161.5 I.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06022492 |
| Source dataset | uspto-grants-2000_02 |
| ORD ID | ord-08b81b1a3c2d436a9ed3634aed1196ad |
| Source note | uspto-grants-2000_02 |