HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Iodoethane | HCID 6340 | — |
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | 2-Chloro-6-(3-fluoro-phenyl-amino)-purine | HCID 21988328 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Lösungsmittel | 1,4-Dioxane--water (1/1) | HCID 21886435 | — |
| Produkt | 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine | HCID 21988319 | — |
Reaktionsschritte
1 g (3.47 mmol) of 2-chloro-6-(3-fluoro-phenyl-amino)-purine, 1.8 g (5.5 mmol) of caesium carbonate and 2.3 ml (27.8 mmol) of iodoethane are stirred in 14 ml of a dioxane/water mixture (4:3) and 12 ml of DMF at RT for 16 h. Thereafter, the reaction mixture is diluted with ethyl acetate and the organic phase is washed with water and dried over sodium sulfate. After removal of the solvent, the residue is chromatographed over silica gel (mobile phase: ethyl acetate/hexane=4:1) and 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine is isolated; m.p. 136° C.; FAB-MS: (M+H)+=292; Rf=0.7 (CH2Cl2:methanol=9:1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07091346B1 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-598185acff304cc3a86a995c03c157bb |
| Quellennotiz | uspto-grants-2006_08 |