HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triphenylphosphine → HCID 66999426, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triphenylphosphine | HCID 11776 | — |
| Edukt | Dibenzyl azodicarboxylate | HCID 5387121 | — |
| Edukt | HCID 66999400 | HCID 66999400 | — |
| Edukt | 5-chloropyridin-2-ol | HCID 178516064 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | HCID 66999426 | HCID 66999426 | 65,2% |
Reaktionsschritte
To a suspension of PPh3 (PPh3 polymer bound, 3 mmol PPh3/g resin) (0.44 g, 1.69 mmol) in THF (50 mL) at 0° C. were added 5-chloro-pyridin-2-ol (0.15 g, 1.15 mmol) and then DBAD (0.28 g, 1.23 mmol). After 5 minutes was added (R)-1-[(3R,4S)-1-benzyl-4-(4-chloro-phenyl)-pyrrolidin-3-yl]-ethanol (0.25 g, 0.79 mmol). The reaction mixture was stirred over night at RT, filtered on celite and concentrated under vacuo. Extraction with EtOAc/aq.NaOH 1M, followed by column chromatography (SiO2, EtOAc/H, 1:3) yielded 0.22 g (65%) of the title compound as a colorless oil. ES-MS m/e: 427.8 (M+H+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08063075B2 |
| Quelldatensatz | uspto-grants-2011_11 |
| ORD ID | ord-89ae718251e14922bfe3195e4722fff2 |
| Quellennotiz | uspto-grants-2011_11 |