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2-Fluorobenzoyl chloride → 2-Fluorobenzoic acid, 2-(4-(trifluoromethyl)phenyl)hydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Fluorobenzoyl chloride | HCID 9808 | — |
| 反応物 | 4-(Trifluoromethyl)phenylhydrazine | HCID 136200 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 2-Fluorobenzoic acid, 2-(4-(trifluoromethyl)phenyl)hydrazide | HCID 15117047 | 85% |
反応手順
To a stirred solution of 75.0 g of 4-(trifluoromethyl)-phenylhydrazine in 500 ml of dry pyridine, cooled in an ice bath, was added dropwise, under nitrogen, 79.1 g of 2-fluorobenzoyl chloride. Upon completion of the addition, the ice bath was removed and the reaction mixture stirred at ambient temperature for 4 hours. The mixture was poured into water and a precipitate formed. Recrystallization of the precipitate from isopropyl alcohol-water, gave 108 g (84%) of 2-fluorobenzoic acid, 2-(4-(trifluoromethyl)phenyl)hydrazide as a solid. Subsequent recrystallization from isopropyl alcohol-water gave the analytical sample, mp 163°-165°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04999356 |
| 出典データセット | uspto-grants-1991_03 |
| ORD ID | ord-84092de639474d16a10f7b220f423f39 |
| 出典メモ | uspto-grants-1991_03 |