化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → Benzoic acid N'-(2-9H-fluoren-9-yl-acetyl)-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 | Fluorene-9-acetic acid | HCID 94852 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Benzoic acid N'-(2-9H-fluoren-9-yl-acetyl)-N'-isopropyl-hydrazide | HCID 57560117 | 40.4% |
反応手順
A solution of 9-fluoreneacetic acid (126 mg, 0.56 mmoles) and benzoic acid N′-isopropyl-hydrazide (100 mg, 0.56 mmoles) in DMF (5 mL) was treated with triethylamine (0.23 mL, 1.68 mmol), HOBT (91 mg, 0.67 mmoles) and EDCI (129 mg, 0.67 mmol) at room temperature for 72 h. The reaction mixture was partitioned between water and dichloromethane. The organic layer was washed with water and brine, then dried over sodium sulfate, filtered and concentrated. The crude was absorbed on silica and purified on a silica gel column with a 10-30% ethyl acetate/hexanes gradient to afford the product as a solid (87 mg, 40%). LC-MS m/e 385.19 (M+H+)
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-3d7adb47e45b4550bc5045491a132aa7 |
| 出典メモ | uspto-grants-2009_02 |