関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | [2-Amino-5-(trifluoromethyl)benzyl][3,5-bis(trifluoromethyl)benzyl]amine | HCID 59343853 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-[2-amino-5-(trifluoromethyl)benzyl]-N-[3,5-bis(trifluoromethyl)benzyl]-acetamide | HCID 86615399 | — |
反応手順
To a solution of [2-amino-5-(trifluoromethyl)benzyl][3,5-bis(trifluoromethyl)benzyl]amine (Example 3) (270 mg, 0.65 mmol) in methylene chloride at 0° C., acetic anhydride (0.061 mL, 0.65 mmol) in methylene chloride and then triethylamine were added (0.018 mL, 0.13 mmol). The solution was stirred for 0.5 hours at 0° C. This solution was washed with saturated sodium bicarbonate, dried over anhydrous sodium sulfate, filtered and concentrated. The title compound was purified by column chromatography using 40% EtOAC/hexane. 1H NMR (CDCl3, 500 MHz) δ 7.80 (s, 1H), 7.56 (s, 2H), 7.30 (d, J=8.5 Hz, 1H), 7.04 (s, 1H), 6.65 (d, J=8.5 Hz, 1H), 4.67 (s, 2H), 4.65 (s, 2H), 2.22 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08193365B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-43cb55cda16947f7ad9e532bed38d8e7 |
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| 出典メモ | uspto-grants-2012_06 |
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