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2-Chlorobenzoyl chloride → 2-Chloro-benzoic acid N'-(5-fluoro-pyridin-2-yl)-hydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Chlorobenzoyl chloride | HCID 69110 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 5-Fluoro-2-hydrazinylpyridine | HCID 19916786 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloro-benzoic acid N'-(5-fluoro-pyridin-2-yl)-hydrazide | HCID 86686722 | 93% |
反応手順
To a solution of (5-fluoro-pyridin-2-yl)-hydrazine (for reference procedure see WO 2010/022076, which is incorporated herein by reference; 1.0 g, 7.87 mmol) and 2-chloro-benzoyl chloride (1 mL, 7.87 mmol) in DCM (50 mL) was added dropwise DIPEA (2.74 mL, 15.75 mmol). The reaction mixture was stirred at RT for 1 h then washed with water. The organic layer was dried through a phase separator and then concentrated in vacuo to afford the title compound (1.95 g, 93%) as a brown solid. LCMS (Method 3): Rt 2.82 min, m/z 266 [MH+].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08835431B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-b1fa1cc4ea254d9abf5af72b3c28aaca |
| 出典メモ | uspto-grants-2014_09 |