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Methyl iodide → 2-Chloro-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 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloro-7H-pyrrolo[2,3-d]pyrimidine | HCID 5706774 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Chloro-7-methyl-7H-pyrrolo(2,3-d)pyrimidine | HCID 57415888 | 59.7% |
反応手順
To a solution of NaH (106.6 mg, 2.67 mmol) in THF (5 mL) was added 2-chloro-7H-pyrrolo[2,3-d]pyrimidine (500 mg, 2.54 mmol) at 0° C. and stirred for 30 minutes at the same temperature. CH3I (1.5 g, 10.2 mmol) was added at 0° C. and the combined mixture stirred for 3 h at 15° C. After TLC showed the reaction was complete, the mixture was diluted with water 20 mL) and extracted with ethyl acetate EA (2×20 mL) and the combined organic layers were washed with brine (30 mL), dried over Na2SO4 and concentrated to give the title compound (254 mg, 47.4%) as colorless oil which was used in next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09388173B2 |
| 出典データセット | uspto-grants-2016_07 |
| ORD ID | ord-d4f396a6a4cd462b933d766abc1c53cb |
| 出典メモ | uspto-grants-2016_07 |