HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → 6-{(SR)-1-[(3RS,4SR)-1-Benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | Dibenzyl azodicarboxylate | HCID 5387121 | — |
| Reactant | 6-Hydroxynicotinonitrile | HCID 7062197 | — |
| Reactant | (RS)-1-[(3RS,4SR)-1-benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanol | HCID 66999712 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 6-{(SR)-1-[(3RS,4SR)-1-Benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethoxy}-nicotinonitrile | HCID 66999403 | 66.3% |
Reaction Steps
To a suspension of PPh3 (PPh3 polymer bound, 3 mmol PPh3/g resin) (1.97 g) in THF (300 mL) at 0° C. were added 6-hydroxy-nicotinonitrile (0.61 g, 5.1 mmol) and then DBAD (1.10 g). After 5 minutes was added (RS)-1-[(3RS,4SR)-1-benzyl-4-(3,4-dichloro-phenyl)-pyrrolidin-3-yl]-ethanol (1.20 g, 3.4 mmol, described herein above). 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, 1:4) yielded 1.02 g (66%) of the title compound as a colorless oil. ES-MS m/e: 452.0 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07812021B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-1cf780ba79124d13a0c69393b818bf76 |
| Source note | uspto-grants-2010_10 |