HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
4-(Trifluoromethoxy)aniline → 2-(4-Trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decane-1,7-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 4-(Trifluoromethoxy)aniline | HCID 600848 | — |
| Edukt | Dimethylalumanylium chloride | HCID 16686359 | — |
| Edukt | 4-(2-Methoxy-ethyl)-2-oxo-piperidine-4-carboxylic acid ethyl ester | HCID 58478414 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Lösungsmittel | Hexane | HCID 8058 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 2-(4-Trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decane-1,7-dione | HCID 58478411 | — |
Reaktionsschritte
4-(2-Methoxy-ethyl)-2-oxo-piperidine-4-carboxylic acid ethyl ester (2 g) and 4-(trifluormethoxy)aniline (3.09 g) were dissolved in toluene (100 ml) under an argon atmosphere at RT, dimethylaluminium chloride in hexane (1 molar, 39.25 ml) was added and the mixture was refluxed for 8 hours. The reaction mixture was then cooled to RT, diluted with AcOEt, quenched with water (9 ml), dried over MgSO4, filtered and the solvent was evaporated off. The residue was adsorbed on silica gel and purified by flash chromatography on silica gel (acetone/CH2Cl2, gradient from 0 to 40%) to give 2-(4-trifluoromethoxy-phenyl)-2,8-diaza-spiro[4.5]decane-1,7-dione as light brown solid. MS (ESI): 329.1 (MH+).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08097634B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-716235da5c764bd5911ca7ef5b43de48 |
| Quellennotiz | uspto-grants-2012_01 |