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Triethylamine → (6-Chloropyridin-3-yl)methyl methanesulphonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | (6-Chloropyridin-3-yl)methanol | HCID 177161 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (6-Chloropyridin-3-yl)methyl methanesulphonate | HCID 23020401 | 88.5% |
反応手順
To a solution of (6-chloro-3-pyridyl)methanol (4.5 g, 31.3 mmol) and triethylamine (13.2 ml, 94.7 mmol) in dichloromethane (90 ml) was dropwise added methanesulfonyl chloride (3.6 ml, 46.5 mmol) over 45 minutes at −9° C. to 4° C. under an atmosphere of nitrogen gas, followed by stirring as it was. After 1 hour, the reaction mixture was elevated to room temperature. The reaction mixture was washed with an aqueous saturated sodium bicarbonate solution and a saturated aqueous ammonium chloride solution, dried over anhydrous sodium sulfate and concentrated, to give the title compound (6.14 g, 88%) as a pale brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07396836B2 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-c17b9e1d63354a7ead1b8e633c251f3c |
| 出典メモ | uspto-grants-2008_07 |