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Iodoethane → 2-chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 2-Chloro-6-(3-trifluoromethyl-phenyl-amino)-purine | HCID 21988237 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | DMF dioxane water | HCID 86622776 | — |
| 生成物 | 2-chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine | HCID 21988187 | — |
反応手順
A mixture comprising 1 g (3.2 mmol) of 2-chloro-6-(3-trifluoromethyl-phenyl-amino)-purine, 1.7 g (5.1 mmol) of caesium carbonate and 2.1 ml (25.6 mmol) of ethyl iodide in 7 ml of dioxane/water/DMF (8:2:2) is stirred at RT for 18 h. It is then diluted with ethyl acetate and the organic phase is washed with water. This phase is separated off and dried over sodium sulfate. After removal of the solvent, the residue is recrystallized from ethyl acetate and diethyl ether. 2-Chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine is obtained; m.p. 129–130° C.; FAB-MS: (M+H)+=342; Rf=0.6 (methylene chloride: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-bf83831a158f40d799e226584860bcea |
| 出典メモ | uspto-grants-2006_08 |