HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloroacetophenone → (S)-1-(2-oxo-2-phenyl-ethyl)-3-(2-phenyl-2-phenylamino-acetoxy)-1-azonia-bicyclo[2.2.2]octane chloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloroacetophenone | HCID 10757 | — |
| Reactant | (S)-quinuclidin-3-yl 2-phenyl-2-(phenylamino)acetate | HCID 59401267 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | (S)-1-(2-oxo-2-phenyl-ethyl)-3-(2-phenyl-2-phenylamino-acetoxy)-1-azonia-bicyclo[2.2.2]octane chloride | HCID 86643222 | 65% |
Reaction Steps
To a solution of (S)-quinuclidin-3-yl 2-phenyl-2-(phenylamino)acetate (50.0 mg, 0.15 mmol) in EtOAc (2 mL), is added 2-chloro-1-phenylethanone (23.0 mg, 0.15 mmol) and the reaction is stirred first at RT for 15 hours, then at 70° C. for 7 hours and finally at RT for 3 days. The solvent is removed and the resulting crude is triturated with i-Pr2O/Et2O (3/1) and then with i-Pr2O to achieve the title compound as a beige solid (47.7 mg, 65% yield, chloride salt, mixture of diastereoisomers).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08455646B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-d9882a7d80e5456089e36c42af36da79 |
| Source note | uspto-grants-2013_06 |