化工社化工社 化学情報印刷レポート · 研究参考用
Phosphorus pentachloride → N-(4-bromophenyl)-2-chloro-6-fluorobenzenecarbohydrazonoyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | 4-bromo-N-[(E)-(2-chloro-6-fluorophenyl)methylideneamino]aniline | HCID 90033658 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | N-(4-bromophenyl)-2-chloro-6-fluorobenzenecarbohydrazonoyl chloride | HCID 131733232 | 23% |
反応手順
To a solution of (2E)-1-(4-bromophenyl)-2-(2-chloro-6-fluorobenzylidene) hydrazine (0.300 g, 1.32 mmol) in benzene (10 mL) was added PCl5 (0.330 g, 1.58 mmol). The reaction mixture was stirred at RT for 18 h. The reaction mass was quenched in water, neutralized with NaHCO3 and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulphate and concentrated to afford 0.110 g of the desired product. 1H NMR (300 MHz, DMSO d6): δ 7.17 (d, J=8.7 Hz, 2H), 7.41 (d, J=8.7 Hz, 3H), 7.45-7.61 (m, 2H), 10.26 (s, 1H). MS (m/z): 361.34 (M−H)−.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09439890B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-fe0ebf7c51b74e4b90c8a8e283a91012 |
| 出典メモ | uspto-grants-2016_09 |