HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ammonia → Diphenyliodonium camphorsulfonate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ammonia | HCID 222 | — |
| Edukt | Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)- | HCID 18462 | — |
| Edukt | Diphenyliodonium dimethylphosphate | HCID 22995015 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | Diphenyliodonium camphorsulfonate | HCID 21930806 | 91% |
Reaktionsschritte
Diphenyliodonium dimethylphosphate (315 mg; 1 mmol) and camphorsulfonic acid (254 mg; 1.1 mmol) were dissolved in methylene chloride (10 ml), and the resultant mixture was stirred, followed by addition of 1% aqueous ammonia (10 ml). After the alkalinity of the solution was confirmed, the solution was stirred vigorously. The thus-obtained mixture was allowed to stand, and the aqueous layer was separated. The aqueous layer was washed with water successively until the aqueous layer exhibited neutral pH. The methylene chloride solution was dried, and the solvent was removed through distillation. The residue was washed in ether by stirring, to thereby precipitate 465 mg of the target compound as white crystals (yield: 91%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07335787B2 |
| Quelldatensatz | uspto-grants-2008_02 |
| ORD ID | ord-9cf36eb79f9545c3ba6d49706b72b75b |
| Quellennotiz | uspto-grants-2008_02 |