HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dicyclohexylcarbodiimide → HCID 58556953, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 3-Quinuclidinol, (-)- | HCID 91404 | — |
| Reactant | [(4-Fluoro-phenyl)-methyl-amino]-phenyl-acetic acid hydrochloride | HCID 67124664 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 58556953 | HCID 58556953 | 84% |
Reaction Steps
PS-DCC (1.02 g, 1.35 mmol, loading: 1.33 mmol/g) is suspended in dry THF (13.5 mL). Then HOBT (0.21 g, 1.35 mmol), [(4-fluoro-phenyl)-methyl-amino]-phenyl-acetic acid hydrochloride (I71) (0.20 g, 0.68 mmol) and (R)-quinuclidin-3-ol (0.26 g, 2.03 mmol) are added. The mixture is shaken at RT overnight. PS-DCC is filtered off, washed with EtOAc and THF. The solution is evaporated and the residue is portioned between EtOAc and water. The organic phase is washed with sat. NaHCO3, dried (Na2SO4) and evaporated. The crude is purified by flash chromatography (DCM/MeOH=95/5) to afford the title compound as a colorless oil (209 mg, 84% yield, mixture of diastereoisomers).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08455646B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-fdc6e6786dd94442a9646c8c61433434 |
| Source note | uspto-grants-2013_06 |