HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Isopropyl iodide → 2-Chloro-9-isopropyl-6-(4-nitro-phenyl-amino)-9H-purine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Isopropyl iodide | HCID 6362 | — |
| Edukt | Cesium carbonate | HCID 10796 | — |
| Edukt | 1,4-Dioxane | HCID 31275 | — |
| Edukt | 2-Chloro-6-(4-nitro-phenyl-amino)-purine | HCID 21988260 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 2-Chloro-9-isopropyl-6-(4-nitro-phenyl-amino)-9H-purine | HCID 21988191 | — |
Reaktionsschritte
A mixture comprising 0.87 g (3 mmol) of 2-chloro-6-(4-nitro-phenyl-amino)-purine, 0.15 g (4.5 mmol) of caesium carbonate and 1.8 ml (18 mmol) of isopropyl iodide is stirred in 22 ml of a mixture comprising dioxane:water:DMF in a ratio of 2:1:4 at 100° C. for 48 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: CH2Cl2:methanol=9:1). The crystalline precipitate obtained on concentration is filtered off and dried. 2-Chloro-9-isopropyl-6-(4-nitro-phenyl-amino)-9H-purine is obtained; m.p.>260° C.; FAB-MS: (M+H)+=333; Rf=0.8 (CH2Cl2:methanol=9:1).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07091346B1 |
| Quelldatensatz | uspto-grants-2006_08 |
| ORD ID | ord-11beb6d00d1b42dca5407a695e214e9e |
| Quellennotiz | uspto-grants-2006_08 |