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Methyl iodide → 4-chloro-5-iodo-7-methyl-7H-pyrrolo[2,3-d]pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 6-Chloro-7-iodo-7-deazapurine | HCID 14809281 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-chloro-5-iodo-7-methyl-7H-pyrrolo[2,3-d]pyrimidine | HCID 42609462 | 61% |
反応手順
To a mixture of 4-chloro-5-iodo-7H-pyrrolo[2,3-d]pyrimidine (Preparation 225, 30 g, 0.1 mol), Cs2CO3 (50 g, 0.15 mol) in DMF (150 mL), MeI (28.4 g, 0.2 mol) was added dropwise at 0° C. After addition, the mixture was stirred at room temperature for 10 hours. The reaction mixture was cooled to 0° C. and quenched by the addition of water (500 mL). Then the solid was collected by filtration and washed with Et2O (100 mL) to afford 4-chloro-5-iodo-7-methyl-7H-pyrrolo[2,3-d]pyrimidine as a brown solid in 61% yield, 20 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846698B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-5183687992584b168accd678f781f565 |
| 出典メモ | uspto-grants-2014_09 |