関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 1,1-Dibromo-3,3,3-trifluoroacetone | HCID 550523 | — |
| 反応物 | Ethyl 2-chloro-5-hydrazinocinnamate | HCID 54155293 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl 2-chloro-5-(3,3,3-trifluoro-2-oxopropylidenehydrazino)cinnamate | HCID 69141416 | 97.5% |
反応手順
First, 7.4 g (90.2 mmol) of sodium acetate and 8.0 g (28.2 mmol) of 1,1-dibromo-3,3,3-trifluoroacetone were mixed with 70 ml of water, and the mixture was stirred at 80° C. for 30 minutes and then cooled, to which 7.0 g of ethyl 2-chloro-5-hydrazinocinnamate was added at 10° C. or lower, and the mixture was stirred for 3 hours. The precipitated crystals were collected by filtration and dried, which afforded 9.6 g (27.5 mmol) of ethyl 2-chloro-5-(3,3,3-trifluoro-2-oxopropylidenehydrazino)cinnamate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06482773B1 |
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| 出典データセット | uspto-grants-2002_11 |
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| ORD ID | ord-99695bcb3f9e4dbda9adfa34fdf8599e |
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| 出典メモ | uspto-grants-2002_11 |
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