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Isopropyl iodide → 2-Chloro-9-isopropyl-6-(4-nitro-phenyl-amino)-9H-purine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isopropyl iodide | HCID 6362 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1,4-Dioxane | HCID 31275 | — |
| 反応物 | 2-Chloro-6-(4-nitro-phenyl-amino)-purine | HCID 21988260 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Chloro-9-isopropyl-6-(4-nitro-phenyl-amino)-9H-purine | HCID 21988191 | — |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091346B1 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-11beb6d00d1b42dca5407a695e214e9e |
| 出典メモ | uspto-grants-2006_08 |