HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → N-(2-n-Propylpentanoyl)-1-aminoindan
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | 2-Propylvaleryl chloride | HCID 76240 | — |
| Edukt | (+-)-1-Aminoindan | HCID 123445 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | N-(2-n-Propylpentanoyl)-1-aminoindan | HCID 11658951 | 69,3% |
Reaktionsschritte
A solution of valproyl chloride (1.55 g, 9.6 mmole) in toluene (25 ml) was added dropwise to a stirred and ice-cooled solution of 1-aminoindan (1.47 g, 10.0 mmole) and Et3N (1.11 g, 11 mmole) . The mixture was stirred at ambient temperature for 17 hours, EtOAc (60 ml) and water (50 ml) were added and the phases were separated. The organic phase was washed successively with 0.1N HCl (40 ml), 0.1N NaHCO3 (40 ml) and saturated NaCl (40 ml), dried over magnesium sulphate and evaporated to dryness under reduced pressure. The residue was treated with hexane (15 ml, 30 min stirring, RT) and filtered. The crude product was crystallized from hexane:EtOAc (70:30 mixture), to give 1.72 g (6.65 mmole, 69%) of a white crystalline solid, mpt: 133-4° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05994408 |
| Quelldatensatz | uspto-grants-1999_11 |
| ORD ID | ord-c6771f5025c142c88c55c3054a02397a |
| Quellennotiz | uspto-grants-1999_11 |