関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | (Chloromethyl)sulfonyl chloride | HCID 77054 | — |
| 反応物 | Ethanone, 2-amino-1-phenyl-, hydrochloride (1:1) | HCID 2723597 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-(Chloromethylsulfonylamino)acetophenone | HCID 23024417 | 76% |
反応手順
2-Aminoacetophenone hydrochloride (4.56 g, 26.6 mmol) was dissolved in dichloromethane (250 mL). To the solution was added triethylamine (9.30 mL, 66.7 mmol), and the mixture was stirred at room temperature for 10 minutes. After the reaction mixture was cooled to 0° C., chloromethanesulfonyl chloride (purity 90%, 3.60 mL, 36.3 mmol) was added to the mixture, and the mixture was stirred at the same temperature for 1 hour. To the reaction mixture was added 2 mol/L hydrochloric acid, and the mixture was extracted with chloroform. The organic layer was washed with saturated aqueous sodium chloride, and then dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. To the residue was added diethyl ether, and the deposited crystals were collected by filtration and dried to obtain 2-(chloromethylsulfonylamino)acetophenone (5.00 g, 76%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07425636B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-c4419f48247f49d78d5729b8f6dd7492 |
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| 出典メモ | uspto-grants-2008_09 |
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