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2-(Ethylamino)ethanol → 3-Chloro-N-ethyl-2,4-difluoro-N-(2-hydroxyethyl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(Ethylamino)ethanol | HCID 8072 | — |
| 反応物 | 3-Chloro-2,4-difluorobenzoyl chloride | HCID 2773538 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 3-Chloro-N-ethyl-2,4-difluoro-N-(2-hydroxyethyl)benzamide | HCID 57663223 | 83.4% |
反応手順
3-Chloro-2,4-difluorobenzoylchloride (211 mg, 1 mmol) in DCM (1 mL) was added to a stirred solution of 2-(ethylamino)ethanol (98 mg, 1.1 mmol) in a mixture of DCM (1 mL) and 10% sodium hydroxide solution (1 mL) at 0° C. After the addition of the acid chloride was complete, the mixture was warmed to RT and stirred for approximately 4 hours. The two layers were separated and the aqueous layer was extracted with DCM (3×30 mL). The organic layers were combined, dried (MgSO4), filtered and evaporated to give a colourless oil (220 mg). The material was used without further purification or analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07943607B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-27bd019121244aa983971f73c4b2dc9a |
| 出典メモ | uspto-grants-2011_05 |