HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl iodide → 4-[Methyl-(2,2,2-trifluoro-acetyl)-amino]-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl iodide | HCID 6328 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Edukt | 1,2-Pyrrolidinedicarboxylic acid, 4-[(2,2,2-trifluoroacetyl)amino]-, 1-(1,1-dimethylethyl) 2-methyl ester | HCID 87364897 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 4-[Methyl-(2,2,2-trifluoro-acetyl)-amino]-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester | HCID 87365907 | — |
Reaktionsbedingungen
| Temperatur | 80 °C |
|---|
Reaktionsschritte
To a solution of 4-(2,2,2-Trifluoro-acetylamino)-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester 2-methyl ester (0.26 g, 0.76 mmol) in DMF (2 mL) was added potassium carbonate (0.139 g, 1 mmol) followed by methyl iodide (0.14 g, 1 mmol). The reaction mixture was stirred at 80° C. for 16 hours and partitioned between water and ethyl acetate. The ethyl acetate layer was washed with brine, dried over Na2SO4, filtered, and the solvent evaporated in vacuo to yield a crude solid. The crude solid was purified via flash chromatography (50% ethyl acetate in Hexanes) to yield the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08426604B2 |
| Quelldatensatz | uspto-grants-2013_04 |
| ORD ID | ord-81db8254b4834cd1a604db8ecfa20a77 |
| Quellennotiz | uspto-grants-2013_04 |