関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Iodo-p-toluidine | HCID 118889 | — |
| 反応物 | 3-Fluoro-5-(trifluoromethyl)benzoyl chloride | HCID 519364 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-fluoro-N-(3-iodo-4-methylphenyl)-5-(trifluoromethyl)benzamide | HCID 69044093 | — |
反応手順
3-Iodo-4-methylaniline (2.42 g, 10.4 mmol) was dissolved in DCM (20.00 mL) and triethylamine (TEA) (1.70 mL, 12.2 mmol) was added and the resulting mixture was cooled to 0° C. To the mixture was added dropwise 3-fluoro-5-(trifluoromethyl)benzoyl chloride (1.60 mL, 10.5 mmol) and the resulting mixture was stirred at 0° C. for 45 minutes and at 25° C. for 16 hours. The reaction was extracted with ethyl acetate and the organic extracts were washed with water sat. Na2CO3, saturated NaCl, dried (MgSO4) and concentrated in vacuo. The reaction product was used in the next reaction without purification. 1H NMR (CDCl3): δ □ 8.98 (d, 1H), 7.78 (s, 1H), 7.72 (m, 2H), 7.55 (m, 2H), 7.23 (d, 1H), 2.42 (s, 3H). MS (EI) m/z=424 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841318B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-7769b28e24b24870a3907f4a8265b0b7 |
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| 出典メモ | uspto-grants-2014_09 |
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