関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Stannous Chloride | HCID 24479 | — |
| 反応物 | 5-Amino-2-chloro-4-fluorophenol | HCID 158654 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 2-Fluoro-4-chloro-5-hydroxyphenylhydrazine hydrochloride | HCID 69142106 | 352.2% |
反応手順
First, 32.3 g of 5-amino-2-chloro-4-fluorophenol was mixed with 150 ml of concentrated hydrochloric acid, and the mixture was stirred at 50° C. for 30 minutes, to which a solution of 15 g of sodium nitrite dissolved in 40 ml of water was added dropwise at 0° C. over 10 minutes. After stirring at 0° C. for 1 hour, the mixture was cooled to -50° C. Then, a solution of 132 g of tin (II) chloride dissolved in 132 g of concentrated sulfuric acid was rapidly added dropwise at -50° C., and the mixture was gradually warmed to room temperature and stirred for 1 hour. The solids formed were collected by filtration and dried at 80° C. under reduced pressure to give 75 g of the crude 2-fluoro-4-chloro-5-hydroxyphenylhydrazine hydrochloride crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06090753 |
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| 出典データセット | uspto-grants-2000_07 |
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| ORD ID | ord-32abd69c63984df281faf9fc48596faa |
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| 出典メモ | uspto-grants-2000_07 |
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