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Ethylamine hydrochloride → N-Ethyl-2-(4-iodo-phenyl)-propionamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylamine hydrochloride | HCID 11198 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 2-(4-Iodophenyl)propanoic acid | HCID 15225573 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-Ethyl-2-(4-iodo-phenyl)-propionamide | HCID 66693450 | — |
反応手順
1.97 g (7.14 mmol) 2-(4-Iodo-phenyl)-propionic acid (111.1) and 1.25 mL (7.14 mmol) DIPEA are added to 582 mg (7.14 mmol) ethylamine hydrochlorid in 70 mL DCM. 1.64 g (8.57 mmol) N-(3-Dimethylaminopropyl)-N-ethylcarbodiimide hydrochloride and 194 mg (1.43 mmol) 1-hydroxy-7-azabenotriazole are added at 0° C. Subsequently, cooling is removed and the mixture is stirred for 20 h at rt. After that time, the mixture is washed with water and brine, dried over sodium sulphate and the solvent is evaporated. The residue is purified by column chromatography (silicia gel; heptane:EtOAc 50:50).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08877754B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-a3e0281aa7624959a4a5400401d16364 |
| 出典メモ | uspto-grants-2014_11 |