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HRID 133519作成日:2026年10月25日
1,1,1-Trifluoro-2,4-pentanedione → 1-(2-Chloro-6-methyl-4-phenyl-thieno[2,3-b]pyridin-5-yl)-2,2,2-trifluoro-ethanone
https://huagongshe.com/reaction/133519
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,1,1-Trifluoro-2,4-pentanedione | HCID 73943 | — |
| 反応物 | (2-Amino-5-chloro-thiophen-3-yl)-phenyl-methanone | HCID 16640283 | — |
| 触媒 | Sulfuric Acid | HCID 1118 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 1-(2-Chloro-6-methyl-4-phenyl-thieno[2,3-b]pyridin-5-yl)-2,2,2-trifluoro-ethanone | HCID 11544922 | 23% |
反応手順
To a stirred solution of 30 mg (0.13 mmol) (2-amino-5-chloro-thiophen-3-yl)-phenyl-methanone in 2 ml acetic acid was added 0.016 ml (0.13 mmol) of 1,1,1-trifluoro-pentane-2,4-dione and one drop of sulfuric acid. The mixture was then stirred at 70° C. for 10 minutes in a microwave and then concentrated in vacuo. Preparative HPLC (30% CE-CN/H20) afforded 10 mg (23%) 1-(2-chloro-6-methyl-4-phenyl-thieno[2,3-b]pyridin-5-yl)-2,2,2-trifluoro-ethanone as a light brown solid. ES-MS m/e (%): 356 (M+H+, 100).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07390903B2 |
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| 出典データセット | uspto-grants-2008_06 |
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| ORD ID | ord-ab232513225c47fca077c1f40b2a7bec |
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| 出典メモ | uspto-grants-2008_06 |
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