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Triethylamine → benzoic acid N'-[3-(3-bromo-phenyl)-propionyl]-N'-isopropyl-hydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 1-Benzoyl-2-isopropylhydrazine | HCID 18869 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 3-(3-bromophenyl)propanoic Acid | HCID 2063862 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | benzoic acid N'-[3-(3-bromo-phenyl)-propionyl]-N'-isopropyl-hydrazide | HCID 57560133 | 67.2% |
反応手順
A solution of (3-(3-bromophenyl)propionic acid (257 mg, 1.12 mmoles) and benzoic acid N′-isopropyl-hydrazide (200 mg, 1.12 mmoles) in DMF (6 mL) was treated with triethylamine (0.47 mL, 3.36 mmoles), HOBT (182 mg, 1.34 mmoles) and EDCI (2.58 mg, 1.34 mmoles) at room temperature for 18 h. The reaction mixture was partitioned between water and dichloromethane. The organic layer was washed with brine, dried over sodium sulfate, filtered and concentrated. The crude was absorbed on silica and purified on a silica gel column with a 20-40% ethyl acetate/hexanes gradient to afford the product as a solid (293 mg, 67%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07485752B2 |
| 出典データセット | uspto-grants-2009_02 |
| ORD ID | ord-c5ce0e9a4c4b4820b85654d5e825840b |
| 出典メモ | uspto-grants-2009_02 |