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2-(Methylamino)ethanol → 3-chloro-2,4-difluoro-N-(2-hydroxyethyl)-N-methylbenzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(Methylamino)ethanol | HCID 8016 | — |
| 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-2,4-difluoro-N-(2-hydroxyethyl)-N-methylbenzamide | HCID 57663213 | 61% |
反応手順
3-Chloro-2,4-difluorobenzoylchloride (CAS no. 157373-00-7) (211 mg, 1 mmol) in DCM (1 mL) was added to a stirred solution of 2-(methylamino)ethanol (83 mg, 1.1 mmol) in a mixture of DCM (1 mL) and 10% sodium hydroxide solution (1 mL) at 0° C. The mixture was warmed to room temperature 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 afford the product (180 mg, 61%). 1H NMR δ (400 MHz, CDCl3): 3.01 (s, 3H), 3.37 (t, 1H), 3.74 (t, 2H), 3.92 (t, 2H), 7.06 (td, 1H), 7.28-7.37 (m, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07902200B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-a98733b8ffdf4d08ba239b9b286180a9 |
| 出典メモ | uspto-grants-2011_03 |