関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | (4-Chloro-2-fluoro-5-propan-2-yloxyphenyl)hydrazine | HCID 185080 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 1,1-Dibromo-3,3,3-trifluoroacetone | HCID 550523 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 3,3,3-Trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone) | HCID 69141430 | — |
反応手順
To a mixed solution of 5.3 g (53.5 mmol) of sodium acetate and about 100 ml of water was added under ice cooling 6.6 g (24.3 mmol) of 1,1-dibromo-3,3,3-trifluoroacetone, and the reaction was allowed to proceed at 70° C. for 20 minutes. Then, the reaction mixture was cooled to room temperature, to which a solution of 5.8 g (21.5 mmol) of 2-fluoro-4-chloro-5-isopropoxyphenylhydrazine dissolved in about 20 ml of diethyl ether was added, and the reaction mixture was stirred at room temperature for 1 hour. The ether layer was separated, washed once with 10 ml of saturated sodium chloride solution, and dried with magnesium sulfate. The diethyl ether was distilled out, which afforded 6.5 g (20.0 mmol) of 3,3,3-trifluoro-2-oxo-propanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06703503B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-285974394a6940eb86913218fa000983 |
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| 出典メモ | uspto-grants-2004_03 |
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